化工进展2017，Vol.36Issue(z1)：402-405,4.DOI:10.16085/j.issn.1000-6613.2017-0085
5-苯基-7-氯-1,3-二氢-2H-1,4-苯并二氮杂(卓)-2-酮的微波合成
Synthesis of 5-phenyl-7-chloro-1 ,3-dihydro-2H-1 ,4-benzodiazepin-2-one under microwave irradiation
吴双双 1陆勇 1王文峰 1胡燕飞 1陈天云1
作者信息
- 1. 合肥工业大学化学与化工学院,安徽 合肥 230009
- 折叠
摘要
Abstract
In this paper,2-amino-5-chloro-benzophenone and chloroacetyl chloride were used as starting materials to synthesize 2-chloroacetylamino-5-chloro-benzophenone by chloroacetylation and then reacted with hexamethylenetetramine under microwave irradiation by Delépine reaction and the ketamine condensation reaction to give 5-phenyl-7-chloro-1 , 3-dihydro-2 H-1 ,4-benzodiazepin-2-one. The influence of the main reaction conditions on the yield of the product was studied by single factor experiment. The optimum reaction conditions were determined as follows: reaction temperature 100℃, n (2-chloroacetylamino-5-chloro-benzophenone ):n(hexamethylenetetramine)=1:2.0,reaction time 50min,2mL of 36% acetic acid,25mL of anhydrous ethanol and the yield of the cyclization reaction reached 89.6% under the optimal reaction conditions,the total yield was 84.8%,The experimental reproducibility is better. The products were characterized by melting point,IR and 1 HNMR. The results showed that the synthesized product was the target product.关键词
5-苯基-7-氯-1,3-二氢-2H-1,4-苯并二氮杂(卓)-2-酮/2-氨基-5氯-二苯甲酮/微波辐射/酰化/环合Key words
5-phenyl-7-chloro-1/3-dihydro-2H-1/4-benzodiazepine-2-one/2-amino-5-chloro-benzophenone/microwave irradiation/chloroacetylation/cyclization分类
化学化工引用本文复制引用
吴双双,陆勇,王文峰,胡燕飞,陈天云..5-苯基-7-氯-1,3-二氢-2H-1,4-苯并二氮杂(卓)-2-酮的微波合成[J].化工进展,2017,36(z1):402-405,4.
