摘要
在综述现有烷基取代环己胺合成方法的基础上,以4,4-二甲基环己胺为例介绍一种优化改进的Leuckart-Wallach反应.优化后的反应以甲醇/氨水9∶1为溶剂体系,10%钯/碳为催化剂,利用甲酸铵为氢源和氮源,一锅法还原胺化4,4-二甲基环己酮得到4,4-二甲基环己胺,该方法产品收率和纯度高,条件温和,操作简便,适用于工业化生产.
A method for the synthesis of alkyl substituted cyclohexan-1-amines was summarized. A new condition for reductive amination of 4,4-dimethylcyclohexan-1-one to form 4,4-dimethylcyclohexan-1-amine by improved Leuckart-Wallach reaction was described. With methanol/ammonium hydroxide（ 9∶ 1） as the solvents and palladium/carbon as a catalyst,the reaction was carried out by using 4,4-dimethylcyclohexan-1-one as a substrate,ammonium formate as a source of nitrogen and hydrogen. The condition of this one-pot reaction was mild with convenient work-up. The yield of target product was higher and the purity of it was better. Accordingly,this method is suitable for industrial production.
出处
《化学研究》
CAS
2017年第1期39-43,共5页
Chemical Research
基金
国家科技重大专项“重大新药创制”(2015ZX09102007-004)
中国医学科学院医学与健康科技创新工程(2016-I2M-3-022)
关键词
4
4-二甲基环己胺
甲醇/氨水
甲酸铵
还原胺化
4
4-dimethylcyclohexan-1-amine
methanol/ammonium hydroxide
ammonium formate
reductive amination
