摘要
以2 甲基 6 乙基苯胺、甲醛、氯乙酰氯和正丁醇等为主要原料,以一种经济环保的工艺路线合成了杀菌剂2 甲基 6 乙基 N 丁氧甲基 N 氯乙酰基苯胺。考察了反应条件对反应结果的影响,获得了较佳的反应条件:烯胺化反应中n(甲醛)/n(2 甲基 6 乙基苯胺)=1 5,反应温度70~75℃,反应时间2h;酰化反应中n(氯乙酰氯)/n(2 甲基 6 乙基苯胺)=1 15,反应温度30~35℃,反应时间1 0h;醚化反应中n(丁醇)/n(2 甲基 6 乙基苯胺)=5 5,反应温度50℃,反应时间5h。在较佳反应条件下,产品质量分数和收率分别达到93%和90%。
A new process for the synthesis of 2-methyl-6-ethyl-N-(butoxymethyl)-N-(chloroacetyl)aniline was studied using formaldehyde,2-methyl-6-ethylaniline,chloroacetyl chloride and butanol as starting materials.In the first step(N-methylenation),n(formaldehyde)/n(2-methyl-6-ethylaniline)=1.5,the reaction temperature is 70~75 ℃,and the reaction time is about 2 h.In the second step(acylation),n(chloroacetyl chloride)/n(2-methyl-6-ethylaniline)=1.15,the reaction temperature is 30~35 ℃,and the reaction time is about 1 h.In the third step(etherification),n(butanol)/n(2-methyl-6-ethylaniline)=5.5,the reaction temperature is 50 ℃,and the reaction time is about 5 h.Under these optimum reaction conditions,the purity and yield of the product were about 93% and 90% respectively.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2004年第z1期153-156,共4页
Fine Chemicals