摘要
以丙烯酸甲酯(MA)与二乙胺为原料,经Michael加成反应、酰胺化反应和热解反应,合成了N,N-二乙基丙烯酰胺(DEAA),考察了工艺条件对各产物收率的影响。结果表明,较佳的Michael加成反应条件为:n(MA)∶n(二乙胺)=1∶1.1,反应温度75℃,反应时间4h,3-二乙基氨基丙酸甲酯收率可达98.7%;较佳的酰胺化反应条件为:n(3-二乙基氨基丙酸甲酯)∶n(二乙胺)=1∶3,m(甲醇钠)∶m(3-二乙基氨基丙酸甲酯)=1∶50,反应温度170℃,反应时间24h,3-二乙基氨基-N,N-二乙基丙酰胺收率可达81.1%;较佳的热解反应条件为:热解温度170℃,热解时间3h,DEAA收率74.4%,分别用FT-IR与1 H NMR对产物结构进行了表征。
N,N-diethylacrylamide（DEAA）was synthesized via Michael addition reaction,amidation reaction and pyrolysis reaction with methyl acrylate（MA）and diethylamine as starting materials.The effects of reaction conditions on each product yield were examined.The results showed that the optimal Michael addition reaction conditions and result were：n（MA）∶n（diethylamine）=1∶1.1,reaction temperature was 75℃,reaction time was 4h,the yield of methyl-3-（diethylamino）propanoate could be up to 98.7%.The optimal amidation reaction conditions and result were：n（methyl-3-（diethylamino）propanoate）：n（diethylamine）=1∶3,m（sodium methoxide）∶m（methyl-3-（diethylamino） propanoate））=1∶50,reaction temperature was 170℃,reaction time was 24h,the yield of 3-（diethylamino）-N,N-diethyl-propanamide could reach 81.1%.The optimal pyrolysis reaction conditions and result were：pyrolysis temperature was 170 ℃,pyrolysis time was 3h,the yield of DEAA was 74.4%.The structure of the product was characterized by FT-IR and 1 H NMR.
出处
《精细石油化工》
CAS
CSCD
北大核心
2013年第4期74-78,共5页
Speciality Petrochemicals
