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一種2?氨基?4?溴?N,5?二甲基苯甲酰胺的合成方法與流程

文檔序號:12341747閱讀:254來源:國知局

本發明公(gong)開了一種2-氨基(ji)(ji)-4-溴-N,5-二甲基(ji)(ji)苯甲酰胺的合成方法(fa),屬(shu)于化學(xue)合成領域(yu)。



背景技術:

近幾年來開(kai)發的(de)(de)一類對(dui)防治(zhi)鱗翅目害(hai)蟲(chong)效果(guo)較(jiao)好的(de)(de)新型殺蟲(chong)劑(ji)為鄰甲酰(xian)氨基苯甲酰(xian)胺,該類殺蟲(chong)劑(ji)因其低毒、低殘留、作用機(ji)制獨特而被廣泛研(yan)究。據報道,該類殺蟲(chong)劑(ji)防治(zhi)害(hai)蟲(chong)的(de)(de)主要原理是活化昆蟲(chong)的(de)(de)魚(yu)尼丁受體。魚(yu)尼丁受體被稱為鈣(gai)通道蛋白,活化昆蟲(chong)的(de)(de)魚(yu)尼丁受體即(ji)使(shi)昆蟲(chong)細胞鈣(gai)離子通道處于(yu)開(kai)放(fang)狀(zhuang)態(tai),導致(zhi)大量(liang)鈣(gai)離子的(de)(de)流失,進而使(shi)昆蟲(chong)的(de)(de)肌肉收縮(suo)直至(zhi)死亡(wang)。



技術實現要素:

本發明提(ti)供一種反應條(tiao)件(jian)溫和、收(shou)率高的(de)2-氨(an)基-4-溴(xiu)-N,5-二甲(jia)基苯(ben)甲(jia)酰(xian)胺的(de)合成方法。

為達到(dao)上述目的(de),本發明(ming)2-氨基(ji)-4-溴-N,5-二甲基(ji)苯甲酰(xian)胺的(de)合成路線為:

本發明涉及的2-氨基(ji)-4-溴-N,5-二甲基(ji)苯甲酰胺(an)的合成過程包括(kuo)以下步驟:

(1)向500mL的四口燒瓶中依次(ci)加入(ru)(ru)120~150mL去離(li)子水(shui)(shui)(shui)、20~22g2-硝基-5-甲(jia)基苯甲(jia)酸、10~12g氫(qing)氧化(hua)鈉(na)、20~22g六水(shui)(shui)(shui)三(san)氯化(hua)鐵和0.1~0.2g鈀,加入(ru)(ru)后將(jiang)四口燒瓶放入(ru)(ru)水(shui)(shui)(shui)浴(yu)鍋(guo)中,升高溫度(du)至75~80℃后向燒瓶中滴(di)加13~15mL質量分數(shu)60%水(shui)(shui)(shui)合(he)肼水(shui)(shui)(shui)溶液,控制滴(di)加速度(du)為3~5mL/min,滴(di)加結束后保(bao)溫攪(jiao)(jiao)拌反(fan)應(ying)5~7h,反(fan)應(ying)結束后冷(leng)卻室溫后將(jiang)反(fan)應(ying)物過濾(lv)(lv)得濾(lv)(lv)液,并用質量分數(shu)20%鹽酸調節濾(lv)(lv)液pH為7.0,調節后的攪(jiao)(jiao)拌60~80min,攪(jiao)(jiao)拌后抽濾(lv)(lv)得濾(lv)(lv)渣,并用去離(li)子水(shui)(shui)(shui)沖洗3~5次(ci)后放入(ru)(ru)烘(hong)箱(xiang)中,在(zai)60~70℃干(gan)燥6~10h,干(gan)燥后得2-氨基-5-甲(jia)基苯甲(jia)酸;

(2)在裝有攪拌(ban)器(qi)、冷凝管(guan)、溫度(du)計(ji)、恒壓滴(di)液漏斗的500mL四口(kou)燒(shao)瓶中加入上(shang)述2-氨(an)基-5-甲基苯(ben)甲酸固(gu)體和200~250mL二氯(lv)甲烷、0.3~0.5mL吡啶,加入后(hou)將四口(kou)燒(shao)瓶放入油浴中,升高(gao)至65~75℃時向燒(shao)瓶中滴(di)加70~80mL質量分數30%二(三(san)氯(lv)甲基)碳酸酯四氫呋(fu)喃(nan)溶(rong)液,控(kong)制滴(di)加速(su)度(du)為1~3mL/min,滴(di)加結束后(hou)保溫攪拌(ban)反應(ying)5~6h,反應(ying)結束后(hou)在800~900W微波功率下加熱至回流,回流20~30min后(hou)冷卻至室溫;

(3)將上(shang)述(shu)冷卻至(zhi)(zhi)室溫(wen)的三口燒(shao)瓶放入(ru)油(you)浴鍋中,升溫(wen)至(zhi)(zhi)55~65℃后(hou)滴(di)加40~50mL質量(liang)分數35%甲胺水溶液,控(kong)制滴(di)加速(su)度為(wei)2~4mL/min,滴(di)加后(hou)保溫(wen)攪拌(ban)反(fan)應(ying)3~5h,反(fan)應(ying)后(hou)將燒(shao)瓶中的反(fan)應(ying)液倒入(ru)分液漏斗中,靜置分層(ceng)后(hou)取上(shang)層(ceng)液,用去離子水洗3~5次后(hou)放入(ru)烘箱中,在50~60℃溫(wen)度下干燥(zao)5~7h,干燥(zao)后(hou)即可(ke)得到2-氨基-N,5-二(er)甲基苯甲酰胺;

(4)將上述2-氨基(ji)-N,5-二甲基(ji)苯(ben)甲酰胺加(jia)(jia)(jia)入(ru)(ru)燒(shao)瓶中(zhong),并(bing)加(jia)(jia)(jia)入(ru)(ru)12~15mL冰醋(cu)酸(suan)、35~40mL去離子(zi)水(shui)(shui),攪拌25~35min后向燒(shao)瓶中(zhong)滴(di)加(jia)(jia)(jia)35~40mL質量分(fen)數(shu)(shu)35%氫(qing)溴酸(suan)溶液(ye)(ye),控制(zhi)滴(di)加(jia)(jia)(jia)速度為5~7mL/min,滴(di)加(jia)(jia)(jia)結束后保溫(wen)攪拌20~30min后放(fang)入(ru)(ru)水(shui)(shui)浴中(zhong),在35~40℃溫(wen)度下向燒(shao)瓶中(zhong)滴(di)加(jia)(jia)(jia)10~12mL質量分(fen)數(shu)(shu)30%雙氧水(shui)(shui),控制(zhi)在10~20min滴(di)加(jia)(jia)(jia)完成,滴(di)加(jia)(jia)(jia)后升溫(wen)至(zhi)50~60℃,攪拌1~3h后加(jia)(jia)(jia)入(ru)(ru)35~40mL去離子(zi)水(shui)(shui)和1.2~1.5g亞硫酸(suan)氫(qing)鈉,攪拌混(hun)合后用質量分(fen)數(shu)(shu)30%氫(qing)氧化鈉溶液(ye)(ye)調(diao)節pH為5.5~6.5,調(diao)節后過濾,得濾渣,用去離子(zi)水(shui)(shui)洗滌(di)3~5次后,放(fang)入(ru)(ru)真空干燥箱中(zhong)在60~80℃溫(wen)度下干燥8~10h,即可得到2-氨基(ji)-4-溴-N,5-二甲基(ji)苯(ben)甲酰胺固體。

具體實施方案

本發明涉及的一(yi)種2-氨基-4-溴-N,5-二(er)甲基苯甲酰胺的合成(cheng)過程(cheng)包括(kuo)以下步驟(zou):

首先向(xiang)(xiang)500mL的(de)四(si)口(kou)燒(shao)瓶(ping)(ping)中(zhong)(zhong)依次加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)120~150mL去離(li)子水、20~22g2-硝(xiao)基(ji)(ji)(ji)(ji)-5-甲(jia)(jia)基(ji)(ji)(ji)(ji)苯(ben)(ben)(ben)甲(jia)(jia)酸(suan)、10~12g氫(qing)氧(yang)化(hua)鈉(na)、20~22g六(liu)水三(san)(san)(san)氯(lv)化(hua)鐵和(he)(he)0.1~0.2g鈀,加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)后(hou)(hou)(hou)將四(si)口(kou)燒(shao)瓶(ping)(ping)放(fang)入(ru)(ru)(ru)(ru)水浴鍋中(zhong)(zhong),升高(gao)溫(wen)(wen)(wen)度(du)(du)(du)至(zhi)(zhi)75~80℃后(hou)(hou)(hou)向(xiang)(xiang)燒(shao)瓶(ping)(ping)中(zhong)(zhong)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)13~15mL質(zhi)量(liang)分(fen)(fen)數(shu)60%水合肼水溶(rong)液(ye)(ye)(ye),控制(zhi)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)速度(du)(du)(du)為(wei)(wei)(wei)(wei)3~5mL/min,滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)結束(shu)(shu)后(hou)(hou)(hou)保溫(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)反(fan)(fan)應5~7h,反(fan)(fan)應結束(shu)(shu)后(hou)(hou)(hou)冷(leng)(leng)(leng)卻室溫(wen)(wen)(wen),將反(fan)(fan)應物過(guo)濾(lv)得(de)(de)(de)(de)濾(lv)液(ye)(ye)(ye),并(bing)用(yong)(yong)質(zhi)量(liang)分(fen)(fen)數(shu)20%鹽酸(suan)調(diao)節濾(lv)液(ye)(ye)(ye)pH為(wei)(wei)(wei)(wei)7.0,調(diao)節后(hou)(hou)(hou)的(de)攪(jiao)(jiao)(jiao)拌(ban)(ban)60~80min,攪(jiao)(jiao)(jiao)拌(ban)(ban)后(hou)(hou)(hou)抽濾(lv)得(de)(de)(de)(de)濾(lv)渣(zha),并(bing)用(yong)(yong)去離(li)子水沖洗3~5次后(hou)(hou)(hou)放(fang)入(ru)(ru)(ru)(ru)烘箱中(zhong)(zhong),在(zai)60~70℃干燥(zao)(zao)6~10h,干燥(zao)(zao)后(hou)(hou)(hou)得(de)(de)(de)(de)2-氨基(ji)(ji)(ji)(ji)-5-甲(jia)(jia)基(ji)(ji)(ji)(ji)苯(ben)(ben)(ben)甲(jia)(jia)酸(suan);在(zai)裝有攪(jiao)(jiao)(jiao)拌(ban)(ban)器、冷(leng)(leng)(leng)凝(ning)管、溫(wen)(wen)(wen)度(du)(du)(du)計、恒(heng)壓滴(di)(di)(di)(di)(di)(di)液(ye)(ye)(ye)漏斗的(de)500mL四(si)口(kou)燒(shao)瓶(ping)(ping)中(zhong)(zhong)加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)上(shang)述2-氨基(ji)(ji)(ji)(ji)-5-甲(jia)(jia)基(ji)(ji)(ji)(ji)苯(ben)(ben)(ben)甲(jia)(jia)酸(suan)固體和(he)(he)200~250mL二(er)氯(lv)甲(jia)(jia)烷和(he)(he)0.3~0.5mL吡啶,加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)后(hou)(hou)(hou)將四(si)口(kou)燒(shao)瓶(ping)(ping)放(fang)入(ru)(ru)(ru)(ru)油浴中(zhong)(zhong),升高(gao)至(zhi)(zhi)65~75℃時向(xiang)(xiang)燒(shao)瓶(ping)(ping)中(zhong)(zhong)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)70~80mL質(zhi)量(liang)分(fen)(fen)數(shu)30%二(er)(三(san)(san)(san)氯(lv)甲(jia)(jia)基(ji)(ji)(ji)(ji))碳(tan)酸(suan)酯四(si)氫(qing)呋(fu)喃溶(rong)液(ye)(ye)(ye),控制(zhi)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)速度(du)(du)(du)為(wei)(wei)(wei)(wei)1~3mL/min,滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)結束(shu)(shu)后(hou)(hou)(hou)保溫(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)反(fan)(fan)應5~6h,反(fan)(fan)應結束(shu)(shu)后(hou)(hou)(hou)在(zai)800~900W微波功(gong)率下加(jia)(jia)(jia)熱至(zhi)(zhi)回流,回流20~30min后(hou)(hou)(hou)冷(leng)(leng)(leng)卻至(zhi)(zhi)室溫(wen)(wen)(wen);將上(shang)述冷(leng)(leng)(leng)卻至(zhi)(zhi)室溫(wen)(wen)(wen)的(de)三(san)(san)(san)口(kou)燒(shao)瓶(ping)(ping)再放(fang)入(ru)(ru)(ru)(ru)油浴鍋中(zhong)(zhong),升溫(wen)(wen)(wen)至(zhi)(zhi)55~65℃后(hou)(hou)(hou)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)40~50mL質(zhi)量(liang)分(fen)(fen)數(shu)35%甲(jia)(jia)胺水溶(rong)液(ye)(ye)(ye),控制(zhi)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)速度(du)(du)(du)為(wei)(wei)(wei)(wei)2~4mL/min,滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)后(hou)(hou)(hou)保溫(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)反(fan)(fan)應3~5h,反(fan)(fan)應后(hou)(hou)(hou)將燒(shao)瓶(ping)(ping)中(zhong)(zhong)的(de)反(fan)(fan)應液(ye)(ye)(ye)倒入(ru)(ru)(ru)(ru)分(fen)(fen)液(ye)(ye)(ye)漏斗中(zhong)(zhong),靜置分(fen)(fen)層后(hou)(hou)(hou)取上(shang)層液(ye)(ye)(ye),用(yong)(yong)去離(li)子水洗3~5次后(hou)(hou)(hou)放(fang)入(ru)(ru)(ru)(ru)烘箱中(zhong)(zhong),在(zai)50~60℃溫(wen)(wen)(wen)度(du)(du)(du)下干燥(zao)(zao)5~7h,干燥(zao)(zao)后(hou)(hou)(hou)即(ji)可(ke)得(de)(de)(de)(de)到(dao)2-氨基(ji)(ji)(ji)(ji)-N,5-二(er)甲(jia)(jia)基(ji)(ji)(ji)(ji)苯(ben)(ben)(ben)甲(jia)(jia)酰(xian)(xian)胺;將上(shang)述制(zhi)備得(de)(de)(de)(de)到(dao)的(de)2-氨基(ji)(ji)(ji)(ji)-N,5-二(er)甲(jia)(jia)基(ji)(ji)(ji)(ji)苯(ben)(ben)(ben)甲(jia)(jia)酰(xian)(xian)胺加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)燒(shao)瓶(ping)(ping)中(zhong)(zhong),并(bing)加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)12~15mL冰醋酸(suan)、35~40mL去離(li)子水,攪(jiao)(jiao)(jiao)拌(ban)(ban)25~35min后(hou)(hou)(hou)向(xiang)(xiang)燒(shao)瓶(ping)(ping)中(zhong)(zhong)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)35~40mL質(zhi)量(liang)分(fen)(fen)數(shu)35%氫(qing)溴酸(suan)溶(rong)液(ye)(ye)(ye),控制(zhi)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)速度(du)(du)(du)為(wei)(wei)(wei)(wei)5~7mL/min,滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)結束(shu)(shu)后(hou)(hou)(hou)保溫(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)20~30min,攪(jiao)(jiao)(jiao)拌(ban)(ban)后(hou)(hou)(hou)放(fang)入(ru)(ru)(ru)(ru)水浴中(zhong)(zhong)在(zai)35~40℃溫(wen)(wen)(wen)度(du)(du)(du)下向(xiang)(xiang)燒(shao)瓶(ping)(ping)中(zhong)(zhong)滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)10~12mL質(zhi)量(liang)分(fen)(fen)數(shu)30%雙氧(yang)水,控制(zhi)在(zai)10~20min滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)完成,滴(di)(di)(di)(di)(di)(di)加(jia)(jia)(jia)后(hou)(hou)(hou)升溫(wen)(wen)(wen)至(zhi)(zhi)50~60℃,攪(jiao)(jiao)(jiao)拌(ban)(ban)1~3h后(hou)(hou)(hou)加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)35~40mL去離(li)子水和(he)(he)1.2~1.5g亞硫酸(suan)氫(qing)鈉(na),攪(jiao)(jiao)(jiao)拌(ban)(ban)混合后(hou)(hou)(hou)用(yong)(yong)質(zhi)量(liang)分(fen)(fen)數(shu)30%氫(qing)氧(yang)化(hua)鈉(na)溶(rong)液(ye)(ye)(ye)調(diao)節pH為(wei)(wei)(wei)(wei)5.5~6.5,調(diao)節后(hou)(hou)(hou)過(guo)濾(lv),得(de)(de)(de)(de)濾(lv)渣(zha),用(yong)(yong)去離(li)子水洗滌3~5次后(hou)(hou)(hou),放(fang)入(ru)(ru)(ru)(ru)真空干燥(zao)(zao)箱中(zhong)(zhong)在(zai)60~80℃溫(wen)(wen)(wen)度(du)(du)(du)下干燥(zao)(zao)8~10h,即(ji)可(ke)得(de)(de)(de)(de)到(dao)2-氨基(ji)(ji)(ji)(ji)-4-溴-N,5-二(er)甲(jia)(jia)基(ji)(ji)(ji)(ji)苯(ben)(ben)(ben)甲(jia)(jia)酰(xian)(xian)胺固體。

實例1

首先向(xiang)(xiang)(xiang)500mL的(de)(de)四(si)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)依(yi)次(ci)(ci)加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)(ru)(ru)120mL去離(li)(li)子(zi)水(shui)(shui)(shui)、20g2-硝基-5-甲(jia)(jia)(jia)(jia)(jia)基苯(ben)甲(jia)(jia)(jia)(jia)(jia)酸(suan)、10g氫氧(yang)化(hua)鈉(na)、20g六水(shui)(shui)(shui)三(san)氯化(hua)鐵和(he)0.1g鈀(ba),加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)(ru)(ru)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)四(si)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)放入(ru)(ru)(ru)(ru)(ru)(ru)水(shui)(shui)(shui)浴(yu)鍋中(zhong)(zhong)(zhong)(zhong),升(sheng)(sheng)(sheng)高(gao)溫(wen)(wen)度(du)(du)(du)至75℃后(hou)(hou)(hou)(hou)(hou)(hou)(hou)向(xiang)(xiang)(xiang)燒(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)滴加(jia)(jia)(jia)13mL質量分(fen)數60%水(shui)(shui)(shui)合(he)肼水(shui)(shui)(shui)溶(rong)液(ye)(ye),控(kong)制(zhi)(zhi)滴加(jia)(jia)(jia)速度(du)(du)(du)為(wei)(wei)3mL/min,滴加(jia)(jia)(jia)結(jie)(jie)(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)保(bao)溫(wen)(wen)攪(jiao)(jiao)拌(ban)(ban)(ban)反(fan)應(ying)(ying)(ying)5h,反(fan)應(ying)(ying)(ying)結(jie)(jie)(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)冷卻(que)(que)室溫(wen)(wen),將(jiang)反(fan)應(ying)(ying)(ying)物過濾(lv)得(de)濾(lv)液(ye)(ye),并用(yong)質量分(fen)數20%鹽(yan)酸(suan)調(diao)節濾(lv)液(ye)(ye)pH為(wei)(wei)7.0,調(diao)節后(hou)(hou)(hou)(hou)(hou)(hou)(hou)的(de)(de)攪(jiao)(jiao)拌(ban)(ban)(ban)60min,攪(jiao)(jiao)拌(ban)(ban)(ban)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)抽濾(lv)得(de)濾(lv)渣,并用(yong)去離(li)(li)子(zi)水(shui)(shui)(shui)沖洗(xi)(xi)3次(ci)(ci)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)放入(ru)(ru)(ru)(ru)(ru)(ru)烘箱(xiang)中(zhong)(zhong)(zhong)(zhong),在60℃干燥(zao)(zao)6h,干燥(zao)(zao)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)得(de)2-氨(an)基-5-甲(jia)(jia)(jia)(jia)(jia)基苯(ben)甲(jia)(jia)(jia)(jia)(jia)酸(suan);在裝有(you)攪(jiao)(jiao)拌(ban)(ban)(ban)器(qi)、冷凝管、溫(wen)(wen)度(du)(du)(du)計(ji)、恒壓滴液(ye)(ye)漏斗的(de)(de)500mL四(si)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)(ru)(ru)上(shang)述(shu)2-氨(an)基-5-甲(jia)(jia)(jia)(jia)(jia)基苯(ben)甲(jia)(jia)(jia)(jia)(jia)酸(suan)固(gu)體(ti)和(he)200mL二(er)氯甲(jia)(jia)(jia)(jia)(jia)烷和(he)0.3mL吡啶,加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)(ru)(ru)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)四(si)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)放入(ru)(ru)(ru)(ru)(ru)(ru)油(you)浴(yu)中(zhong)(zhong)(zhong)(zhong),升(sheng)(sheng)(sheng)高(gao)至65℃時向(xiang)(xiang)(xiang)燒(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)滴加(jia)(jia)(jia)70mL質量分(fen)數30%二(er)(三(san)氯甲(jia)(jia)(jia)(jia)(jia)基)碳酸(suan)酯(zhi)四(si)氫呋喃溶(rong)液(ye)(ye),控(kong)制(zhi)(zhi)滴加(jia)(jia)(jia)速度(du)(du)(du)為(wei)(wei)1mL/min,滴加(jia)(jia)(jia)結(jie)(jie)(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)保(bao)溫(wen)(wen)攪(jiao)(jiao)拌(ban)(ban)(ban)反(fan)應(ying)(ying)(ying)5h,反(fan)應(ying)(ying)(ying)結(jie)(jie)(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)在800W微波功率下(xia)加(jia)(jia)(jia)熱至回流,回流20min后(hou)(hou)(hou)(hou)(hou)(hou)(hou)冷卻(que)(que)至室溫(wen)(wen);將(jiang)上(shang)述(shu)冷卻(que)(que)至室溫(wen)(wen)的(de)(de)三(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)再放入(ru)(ru)(ru)(ru)(ru)(ru)油(you)浴(yu)鍋中(zhong)(zhong)(zhong)(zhong),升(sheng)(sheng)(sheng)溫(wen)(wen)至55℃后(hou)(hou)(hou)(hou)(hou)(hou)(hou)滴加(jia)(jia)(jia)40mL質量分(fen)數35%甲(jia)(jia)(jia)(jia)(jia)胺(an)水(shui)(shui)(shui)溶(rong)液(ye)(ye),控(kong)制(zhi)(zhi)滴加(jia)(jia)(jia)速度(du)(du)(du)為(wei)(wei)2mL/min,滴加(jia)(jia)(jia)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)保(bao)溫(wen)(wen)攪(jiao)(jiao)拌(ban)(ban)(ban)反(fan)應(ying)(ying)(ying)3h,反(fan)應(ying)(ying)(ying)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)燒(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)的(de)(de)反(fan)應(ying)(ying)(ying)液(ye)(ye)倒(dao)入(ru)(ru)(ru)(ru)(ru)(ru)分(fen)液(ye)(ye)漏斗中(zhong)(zhong)(zhong)(zhong),靜置分(fen)層(ceng)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)取上(shang)層(ceng)液(ye)(ye),用(yong)去離(li)(li)子(zi)水(shui)(shui)(shui)洗(xi)(xi)3次(ci)(ci)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)放入(ru)(ru)(ru)(ru)(ru)(ru)烘箱(xiang)中(zhong)(zhong)(zhong)(zhong),在50℃溫(wen)(wen)度(du)(du)(du)下(xia)干燥(zao)(zao)5h,干燥(zao)(zao)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)即可(ke)得(de)到2-氨(an)基-N,5-二(er)甲(jia)(jia)(jia)(jia)(jia)基苯(ben)甲(jia)(jia)(jia)(jia)(jia)酰胺(an);將(jiang)上(shang)述(shu)制(zhi)(zhi)備得(de)到的(de)(de)2-氨(an)基-N,5-二(er)甲(jia)(jia)(jia)(jia)(jia)基苯(ben)甲(jia)(jia)(jia)(jia)(jia)酰胺(an)加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)(ru)(ru)燒(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong),并加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)(ru)(ru)12mL冰醋酸(suan)、35mL去離(li)(li)子(zi)水(shui)(shui)(shui),攪(jiao)(jiao)拌(ban)(ban)(ban)25min后(hou)(hou)(hou)(hou)(hou)(hou)(hou)向(xiang)(xiang)(xiang)燒(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)滴加(jia)(jia)(jia)35mL質量分(fen)數35%氫溴(xiu)酸(suan)溶(rong)液(ye)(ye),控(kong)制(zhi)(zhi)滴加(jia)(jia)(jia)速度(du)(du)(du)為(wei)(wei)5mL/min,滴加(jia)(jia)(jia)結(jie)(jie)(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)保(bao)溫(wen)(wen)攪(jiao)(jiao)拌(ban)(ban)(ban)20min,攪(jiao)(jiao)拌(ban)(ban)(ban)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)放入(ru)(ru)(ru)(ru)(ru)(ru)水(shui)(shui)(shui)浴(yu)中(zhong)(zhong)(zhong)(zhong)在35℃溫(wen)(wen)度(du)(du)(du)下(xia)向(xiang)(xiang)(xiang)燒(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)滴加(jia)(jia)(jia)10mL質量分(fen)數30%雙氧(yang)水(shui)(shui)(shui),控(kong)制(zhi)(zhi)在10min滴加(jia)(jia)(jia)完成,滴加(jia)(jia)(jia)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)升(sheng)(sheng)(sheng)溫(wen)(wen)至50℃,攪(jiao)(jiao)拌(ban)(ban)(ban)1h后(hou)(hou)(hou)(hou)(hou)(hou)(hou)加(jia)(jia)(jia)入(ru)(ru)(ru)(ru)(ru)(ru)35mL去離(li)(li)子(zi)水(shui)(shui)(shui)和(he)1.2g亞硫酸(suan)氫鈉(na),攪(jiao)(jiao)拌(ban)(ban)(ban)混合(he)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)用(yong)質量分(fen)數30%氫氧(yang)化(hua)鈉(na)溶(rong)液(ye)(ye)調(diao)節pH為(wei)(wei)5.5,調(diao)節后(hou)(hou)(hou)(hou)(hou)(hou)(hou)過濾(lv),得(de)濾(lv)渣,用(yong)去離(li)(li)子(zi)水(shui)(shui)(shui)洗(xi)(xi)滌3次(ci)(ci)后(hou)(hou)(hou)(hou)(hou)(hou)(hou),放入(ru)(ru)(ru)(ru)(ru)(ru)真(zhen)空干燥(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)(zhong)在60℃溫(wen)(wen)度(du)(du)(du)下(xia)干燥(zao)(zao)8h,即可(ke)得(de)到2-氨(an)基-4-溴(xiu)-N,5-二(er)甲(jia)(jia)(jia)(jia)(jia)基苯(ben)甲(jia)(jia)(jia)(jia)(jia)酰胺(an)固(gu)體(ti)。

實例2

首(shou)先向(xiang)500mL的(de)(de)四(si)(si)(si)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)依(yi)次加(jia)(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)135mL去(qu)離(li)(li)子(zi)(zi)水(shui)(shui)、21g2-硝基(ji)-5-甲(jia)(jia)(jia)(jia)基(ji)苯(ben)(ben)(ben)甲(jia)(jia)(jia)(jia)酸(suan)(suan)(suan)、11g氫(qing)(qing)氧(yang)化鈉、21g六水(shui)(shui)三(san)氯(lv)(lv)化鐵和(he)0.15g鈀,加(jia)(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)(jiang)四(si)(si)(si)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)放(fang)(fang)入(ru)(ru)水(shui)(shui)浴(yu)鍋中(zhong)(zhong)(zhong),升高溫(wen)(wen)(wen)(wen)(wen)度(du)至(zhi)(zhi)77℃后(hou)(hou)(hou)(hou)(hou)(hou)(hou)向(xiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)14mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)(shu)60%水(shui)(shui)合(he)肼水(shui)(shui)溶(rong)液(ye)(ye)(ye),控(kong)制(zhi)(zhi)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)速(su)度(du)為(wei)4mL/min,滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)結(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)保溫(wen)(wen)(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)反(fan)應(ying)(ying)6h,反(fan)應(ying)(ying)結(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)冷(leng)卻(que)室(shi)溫(wen)(wen)(wen)(wen)(wen),將(jiang)(jiang)反(fan)應(ying)(ying)物過濾(lv)(lv)得(de)(de)(de)濾(lv)(lv)液(ye)(ye)(ye),并(bing)用(yong)質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)(shu)20%鹽酸(suan)(suan)(suan)調節(jie)濾(lv)(lv)液(ye)(ye)(ye)pH為(wei)7.0,調節(jie)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)的(de)(de)攪(jiao)(jiao)(jiao)拌(ban)(ban)70min,攪(jiao)(jiao)(jiao)拌(ban)(ban)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)抽濾(lv)(lv)得(de)(de)(de)濾(lv)(lv)渣(zha),并(bing)用(yong)去(qu)離(li)(li)子(zi)(zi)水(shui)(shui)沖洗4次后(hou)(hou)(hou)(hou)(hou)(hou)(hou)放(fang)(fang)入(ru)(ru)烘箱(xiang)中(zhong)(zhong)(zhong),在(zai)65℃干(gan)(gan)(gan)燥(zao)(zao)8h,干(gan)(gan)(gan)燥(zao)(zao)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)得(de)(de)(de)2-氨基(ji)-5-甲(jia)(jia)(jia)(jia)基(ji)苯(ben)(ben)(ben)甲(jia)(jia)(jia)(jia)酸(suan)(suan)(suan);在(zai)裝(zhuang)有攪(jiao)(jiao)(jiao)拌(ban)(ban)器、冷(leng)凝管、溫(wen)(wen)(wen)(wen)(wen)度(du)計、恒壓(ya)滴(di)(di)液(ye)(ye)(ye)漏斗的(de)(de)500mL四(si)(si)(si)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)上述(shu)2-氨基(ji)-5-甲(jia)(jia)(jia)(jia)基(ji)苯(ben)(ben)(ben)甲(jia)(jia)(jia)(jia)酸(suan)(suan)(suan)固體和(he)225mL二(er)氯(lv)(lv)甲(jia)(jia)(jia)(jia)烷和(he)0.4mL吡啶,加(jia)(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)(jiang)四(si)(si)(si)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)放(fang)(fang)入(ru)(ru)油(you)浴(yu)中(zhong)(zhong)(zhong),升高至(zhi)(zhi)70℃時(shi)向(xiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)75mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)(shu)30%二(er)(三(san)氯(lv)(lv)甲(jia)(jia)(jia)(jia)基(ji))碳酸(suan)(suan)(suan)酯四(si)(si)(si)氫(qing)(qing)呋喃溶(rong)液(ye)(ye)(ye),控(kong)制(zhi)(zhi)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)速(su)度(du)為(wei)2mL/min,滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)結(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)保溫(wen)(wen)(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)反(fan)應(ying)(ying)5.5h,反(fan)應(ying)(ying)結(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)在(zai)800~900W微波(bo)功率下加(jia)(jia)(jia)(jia)(jia)(jia)(jia)熱至(zhi)(zhi)回流,回流25min后(hou)(hou)(hou)(hou)(hou)(hou)(hou)冷(leng)卻(que)至(zhi)(zhi)室(shi)溫(wen)(wen)(wen)(wen)(wen);將(jiang)(jiang)上述(shu)冷(leng)卻(que)至(zhi)(zhi)室(shi)溫(wen)(wen)(wen)(wen)(wen)的(de)(de)三(san)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)再放(fang)(fang)入(ru)(ru)油(you)浴(yu)鍋中(zhong)(zhong)(zhong),升溫(wen)(wen)(wen)(wen)(wen)至(zhi)(zhi)60℃后(hou)(hou)(hou)(hou)(hou)(hou)(hou)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)45mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)(shu)35%甲(jia)(jia)(jia)(jia)胺(an)水(shui)(shui)溶(rong)液(ye)(ye)(ye),控(kong)制(zhi)(zhi)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)速(su)度(du)為(wei)3mL/min,滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)保溫(wen)(wen)(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)反(fan)應(ying)(ying)4h,反(fan)應(ying)(ying)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)(jiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)的(de)(de)反(fan)應(ying)(ying)液(ye)(ye)(ye)倒入(ru)(ru)分(fen)(fen)(fen)液(ye)(ye)(ye)漏斗中(zhong)(zhong)(zhong),靜置分(fen)(fen)(fen)層后(hou)(hou)(hou)(hou)(hou)(hou)(hou)取上層液(ye)(ye)(ye),用(yong)去(qu)離(li)(li)子(zi)(zi)水(shui)(shui)洗3次后(hou)(hou)(hou)(hou)(hou)(hou)(hou)放(fang)(fang)入(ru)(ru)烘箱(xiang)中(zhong)(zhong)(zhong),在(zai)55℃溫(wen)(wen)(wen)(wen)(wen)度(du)下干(gan)(gan)(gan)燥(zao)(zao)6h,干(gan)(gan)(gan)燥(zao)(zao)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)即可得(de)(de)(de)到2-氨基(ji)-N,5-二(er)甲(jia)(jia)(jia)(jia)基(ji)苯(ben)(ben)(ben)甲(jia)(jia)(jia)(jia)酰(xian)胺(an);將(jiang)(jiang)上述(shu)制(zhi)(zhi)備得(de)(de)(de)到的(de)(de)2-氨基(ji)-N,5-二(er)甲(jia)(jia)(jia)(jia)基(ji)苯(ben)(ben)(ben)甲(jia)(jia)(jia)(jia)酰(xian)胺(an)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong),并(bing)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)13mL冰(bing)醋酸(suan)(suan)(suan)、37mL去(qu)離(li)(li)子(zi)(zi)水(shui)(shui),攪(jiao)(jiao)(jiao)拌(ban)(ban)30min后(hou)(hou)(hou)(hou)(hou)(hou)(hou)向(xiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)37mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)(shu)35%氫(qing)(qing)溴酸(suan)(suan)(suan)溶(rong)液(ye)(ye)(ye),控(kong)制(zhi)(zhi)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)速(su)度(du)為(wei)6mL/min,滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)結(jie)束(shu)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)保溫(wen)(wen)(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)25min,攪(jiao)(jiao)(jiao)拌(ban)(ban)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)放(fang)(fang)入(ru)(ru)水(shui)(shui)浴(yu)中(zhong)(zhong)(zhong)在(zai)35~40℃溫(wen)(wen)(wen)(wen)(wen)度(du)下向(xiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)11mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)(shu)30%雙(shuang)氧(yang)水(shui)(shui),控(kong)制(zhi)(zhi)在(zai)15min滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)完成(cheng),滴(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)升溫(wen)(wen)(wen)(wen)(wen)至(zhi)(zhi)55℃,攪(jiao)(jiao)(jiao)拌(ban)(ban)2h后(hou)(hou)(hou)(hou)(hou)(hou)(hou)加(jia)(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)37mL去(qu)離(li)(li)子(zi)(zi)水(shui)(shui)和(he)1.4g亞硫(liu)酸(suan)(suan)(suan)氫(qing)(qing)鈉,攪(jiao)(jiao)(jiao)拌(ban)(ban)混合(he)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)用(yong)質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)(shu)30%氫(qing)(qing)氧(yang)化鈉溶(rong)液(ye)(ye)(ye)調節(jie)pH為(wei)6.0,調節(jie)后(hou)(hou)(hou)(hou)(hou)(hou)(hou)過濾(lv)(lv),得(de)(de)(de)濾(lv)(lv)渣(zha),用(yong)去(qu)離(li)(li)子(zi)(zi)水(shui)(shui)洗滌4次后(hou)(hou)(hou)(hou)(hou)(hou)(hou),放(fang)(fang)入(ru)(ru)真空(kong)干(gan)(gan)(gan)燥(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)在(zai)70℃溫(wen)(wen)(wen)(wen)(wen)度(du)下干(gan)(gan)(gan)燥(zao)(zao)9h,即可得(de)(de)(de)到2-氨基(ji)-4-溴-N,5-二(er)甲(jia)(jia)(jia)(jia)基(ji)苯(ben)(ben)(ben)甲(jia)(jia)(jia)(jia)酰(xian)胺(an)固體。

實例3

首(shou)先向(xiang)(xiang)500mL的(de)四(si)(si)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)依次加(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)150mL去(qu)(qu)離(li)(li)子(zi)(zi)水(shui)、22g2-硝基(ji)-5-甲(jia)(jia)基(ji)苯(ben)(ben)甲(jia)(jia)酸(suan)、12g氫(qing)氧化鈉(na)、22g六(liu)水(shui)三氯化鐵和(he)0.2g鈀,加(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)后(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)(jiang)四(si)(si)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)放(fang)(fang)入(ru)(ru)水(shui)浴(yu)鍋(guo)中(zhong)(zhong)(zhong)(zhong),升高溫(wen)(wen)(wen)(wen)(wen)度(du)(du)至(zhi)80℃后(hou)(hou)(hou)(hou)(hou)(hou)向(xiang)(xiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)15mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)60%水(shui)合肼水(shui)溶(rong)(rong)(rong)(rong)液(ye)(ye),控(kong)(kong)制(zhi)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)速(su)(su)度(du)(du)為(wei)(wei)5mL/min,滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)結(jie)束后(hou)(hou)(hou)(hou)(hou)(hou)保(bao)溫(wen)(wen)(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)反(fan)應(ying)(ying)7h,反(fan)應(ying)(ying)結(jie)束后(hou)(hou)(hou)(hou)(hou)(hou)冷(leng)卻(que)(que)室(shi)溫(wen)(wen)(wen)(wen)(wen),將(jiang)(jiang)反(fan)應(ying)(ying)物過濾得(de)(de)(de)濾液(ye)(ye),并用(yong)質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)20%鹽(yan)酸(suan)調節(jie)(jie)(jie)濾液(ye)(ye)pH為(wei)(wei)7.0,調節(jie)(jie)(jie)后(hou)(hou)(hou)(hou)(hou)(hou)的(de)攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)80min,攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)后(hou)(hou)(hou)(hou)(hou)(hou)抽濾得(de)(de)(de)濾渣,并用(yong)去(qu)(qu)離(li)(li)子(zi)(zi)水(shui)沖洗(xi)3~5次后(hou)(hou)(hou)(hou)(hou)(hou)放(fang)(fang)入(ru)(ru)烘(hong)箱中(zhong)(zhong)(zhong)(zhong),在(zai)70℃干(gan)(gan)(gan)燥(zao)10h,干(gan)(gan)(gan)燥(zao)后(hou)(hou)(hou)(hou)(hou)(hou)得(de)(de)(de)2-氨(an)基(ji)-5-甲(jia)(jia)基(ji)苯(ben)(ben)甲(jia)(jia)酸(suan);在(zai)裝有攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)器、冷(leng)凝(ning)管、溫(wen)(wen)(wen)(wen)(wen)度(du)(du)計、恒(heng)壓滴(di)(di)(di)液(ye)(ye)漏斗的(de)500mL四(si)(si)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)加(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)上(shang)(shang)述2-氨(an)基(ji)-5-甲(jia)(jia)基(ji)苯(ben)(ben)甲(jia)(jia)酸(suan)固體和(he)250mL二(er)(er)氯甲(jia)(jia)烷和(he)0.5mL吡(bi)啶(ding),加(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)后(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)(jiang)四(si)(si)口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)放(fang)(fang)入(ru)(ru)油浴(yu)中(zhong)(zhong)(zhong)(zhong),升高至(zhi)75℃時向(xiang)(xiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)80mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)30%二(er)(er)(三氯甲(jia)(jia)基(ji))碳酸(suan)酯四(si)(si)氫(qing)呋(fu)喃溶(rong)(rong)(rong)(rong)液(ye)(ye),控(kong)(kong)制(zhi)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)速(su)(su)度(du)(du)為(wei)(wei)3mL/min,滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)結(jie)束后(hou)(hou)(hou)(hou)(hou)(hou)保(bao)溫(wen)(wen)(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)反(fan)應(ying)(ying)6h,反(fan)應(ying)(ying)結(jie)束后(hou)(hou)(hou)(hou)(hou)(hou)在(zai)900W微波(bo)功(gong)率下加(jia)(jia)(jia)(jia)(jia)(jia)熱至(zhi)回(hui)流,回(hui)流30min后(hou)(hou)(hou)(hou)(hou)(hou)冷(leng)卻(que)(que)至(zhi)室(shi)溫(wen)(wen)(wen)(wen)(wen);將(jiang)(jiang)上(shang)(shang)述冷(leng)卻(que)(que)至(zhi)室(shi)溫(wen)(wen)(wen)(wen)(wen)的(de)三口燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)再放(fang)(fang)入(ru)(ru)油浴(yu)鍋(guo)中(zhong)(zhong)(zhong)(zhong),升溫(wen)(wen)(wen)(wen)(wen)至(zhi)65℃后(hou)(hou)(hou)(hou)(hou)(hou)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)50mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)35%甲(jia)(jia)胺水(shui)溶(rong)(rong)(rong)(rong)液(ye)(ye),控(kong)(kong)制(zhi)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)速(su)(su)度(du)(du)為(wei)(wei)4mL/min,滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)后(hou)(hou)(hou)(hou)(hou)(hou)保(bao)溫(wen)(wen)(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)反(fan)應(ying)(ying)5h,反(fan)應(ying)(ying)后(hou)(hou)(hou)(hou)(hou)(hou)將(jiang)(jiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)的(de)反(fan)應(ying)(ying)液(ye)(ye)倒(dao)入(ru)(ru)分(fen)(fen)(fen)液(ye)(ye)漏斗中(zhong)(zhong)(zhong)(zhong),靜置分(fen)(fen)(fen)層后(hou)(hou)(hou)(hou)(hou)(hou)取上(shang)(shang)層液(ye)(ye),用(yong)去(qu)(qu)離(li)(li)子(zi)(zi)水(shui)洗(xi)5次后(hou)(hou)(hou)(hou)(hou)(hou)放(fang)(fang)入(ru)(ru)烘(hong)箱中(zhong)(zhong)(zhong)(zhong),在(zai)60℃溫(wen)(wen)(wen)(wen)(wen)度(du)(du)下干(gan)(gan)(gan)燥(zao)7h,干(gan)(gan)(gan)燥(zao)后(hou)(hou)(hou)(hou)(hou)(hou)即可(ke)得(de)(de)(de)到2-氨(an)基(ji)-N,5-二(er)(er)甲(jia)(jia)基(ji)苯(ben)(ben)甲(jia)(jia)酰胺;將(jiang)(jiang)上(shang)(shang)述制(zhi)備得(de)(de)(de)到的(de)2-氨(an)基(ji)-N,5-二(er)(er)甲(jia)(jia)基(ji)苯(ben)(ben)甲(jia)(jia)酰胺加(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong),并加(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)15mL冰醋酸(suan)、40mL去(qu)(qu)離(li)(li)子(zi)(zi)水(shui),攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)35min后(hou)(hou)(hou)(hou)(hou)(hou)向(xiang)(xiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)40mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)35%氫(qing)溴酸(suan)溶(rong)(rong)(rong)(rong)液(ye)(ye),控(kong)(kong)制(zhi)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)速(su)(su)度(du)(du)為(wei)(wei)7mL/min,滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)結(jie)束后(hou)(hou)(hou)(hou)(hou)(hou)保(bao)溫(wen)(wen)(wen)(wen)(wen)攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)30min,攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)后(hou)(hou)(hou)(hou)(hou)(hou)放(fang)(fang)入(ru)(ru)水(shui)浴(yu)中(zhong)(zhong)(zhong)(zhong)在(zai)40℃溫(wen)(wen)(wen)(wen)(wen)度(du)(du)下向(xiang)(xiang)燒(shao)(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)12mL質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)30%雙(shuang)氧水(shui),控(kong)(kong)制(zhi)在(zai)10~20min滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)完成,滴(di)(di)(di)加(jia)(jia)(jia)(jia)(jia)(jia)后(hou)(hou)(hou)(hou)(hou)(hou)升溫(wen)(wen)(wen)(wen)(wen)至(zhi)60℃,攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)3h后(hou)(hou)(hou)(hou)(hou)(hou)加(jia)(jia)(jia)(jia)(jia)(jia)入(ru)(ru)40mL去(qu)(qu)離(li)(li)子(zi)(zi)水(shui)和(he)1.5g亞硫酸(suan)氫(qing)鈉(na),攪(jiao)(jiao)(jiao)拌(ban)(ban)(ban)(ban)(ban)混合后(hou)(hou)(hou)(hou)(hou)(hou)用(yong)質量(liang)(liang)分(fen)(fen)(fen)數(shu)(shu)(shu)30%氫(qing)氧化鈉(na)溶(rong)(rong)(rong)(rong)液(ye)(ye)調節(jie)(jie)(jie)pH為(wei)(wei)6.5,調節(jie)(jie)(jie)后(hou)(hou)(hou)(hou)(hou)(hou)過濾,得(de)(de)(de)濾渣,用(yong)去(qu)(qu)離(li)(li)子(zi)(zi)水(shui)洗(xi)滌(di)5次后(hou)(hou)(hou)(hou)(hou)(hou),放(fang)(fang)入(ru)(ru)真空干(gan)(gan)(gan)燥(zao)箱中(zhong)(zhong)(zhong)(zhong)在(zai)80℃溫(wen)(wen)(wen)(wen)(wen)度(du)(du)下干(gan)(gan)(gan)燥(zao)10h,即可(ke)得(de)(de)(de)到2-氨(an)基(ji)-4-溴-N,5-二(er)(er)甲(jia)(jia)基(ji)苯(ben)(ben)甲(jia)(jia)酰胺固體。

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