摘要
S-环氧氯丙烷与氨水和苯甲醛反应,酸性水解后,4-二甲氨基吡啶作为催化剂,醋酐作为酰化试剂合成(S)-N-(2-乙酰氧基-3-氯丙基)乙酰胺。用LC-MS分析S-环氧氯丙烷与氨水反应的副产物,发现在氨水中加入醋酸铵可以抑制副反应,提高1-氨基-3-氯-2-丙醇的收率;在4-二甲氨基吡啶催化下与乙酸酐反应得到(S)-N-(2-乙酰氧基-3-氯丙基)乙酰胺,收率90.91%,时间缩短了4h。
（S）-N-[-2-acetoxy-3-chloropropyl-] acetamide was synthesized from （S）-（ ＋ ）-epichloro- hydrin through three steps, including ring cleavage in ammonium hydroxide, hydrolysis under diluted acid, and acylation with acetic anhydride as an acylating agent. The by-products of the reaction of （S）-（＋）-Epichlorohydrin with aqueous ammoniawere analyzed with LC-MS and side reactions were suppressed by the addition of ammonium acetate. The yield of （S）-N-（2-acetoxy-3-chloropropyl） acet- amidewas increased to 90.91% and the reaction time was shortened by 4 hours under catalyst of 4- dimethylaminopyridine.
出处
《精细石油化工》
CAS
CSCD
北大核心
2016年第5期61-64,共4页
Speciality Petrochemicals
基金
国家海洋公益性行业科研专项(201305007)
江苏省六大人才高峰资助项目(2009年
2013年)
江苏省海洋资源开发研究院科研项目(JSIMR201409)
连云港市工业攻关项目(CG1508)
