摘要
以1,3-溴氯丙烷和二甲胺为原料制备N,N-二甲氨基氯丙烷盐酸盐,通过调整反应投料比(二甲胺:1,3-溴氯丙烷=1.05:1),改进反应的后处理,以及用异丙醇重结晶,可以方便地得到产品盐,其纯度为99.3%(HPLC示差折光分析法),收率为87.1%.甲苯及未反应的原料可以方便地回收再使用.对工艺中的主要杂质进行分析,结构确证为N,N,N’,N’-四甲基丙二胺.
N, N - dimethylaminochloropropane is obtained from 1 - bromo - 3 - chloropropane and dimethylamine. The molar ratio of dimethyl amine and 1 - bromo - 3 - chloropropane has been adjusted to be 1.05 ： 1. The product salt can be easily purified by isopropanol recrystallization, and the final yield is 87.1% with the purity of 99.3 % （ HPLC - RID method）. Toluene and unreacted 1 - bromo - 3 - chloropropane can be recovered and reused conveniently. N, N, N＇, N＇ - tetramethylpropylenediamine has been confirmed to be the principal impurity occurring in this technique.
出处
《绍兴文理学院学报》
2010年第7期29-31,共3页
Journal of Shaoxing University
关键词
1
3-溴氯丙烷
二甲胺
N
N-二甲氨基氯丙烷盐酸盐
N
N
N'
N'-四甲基丙二胺盐酸盐
1 - bromo - 3 - chloropropane
dimethyl amine
N, N - dimethylaminochloropropane hydrochloride
N, N, N＇, N＇ - tetramethylpropylenediamine hydrochloride
