HRID410365
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
To a solution of 1-benzyl-1,3-dihydro-benzoimidazol-2-ylideneamine (247 mg, 1.10 mmol) in 2-butanone (40 ml) was added 3-(3-chloro-propoxy)-benzoic acid ethyl ester (0.40 g, 1.65 mmol) and KI (0.55 g, 3.32 mmol). The reaction was heated to 85° C. where it was maintained for 54 h. After this time, the mixture was cooled to rt and filtered. The filtrate was concentrated under reduced pressure and combined with the collected solid, washed with diethyl ether and petroleum ether and dried to provide 3-[3-(3-benzyl-2-imino-2,3-dihydro-benzoimidazol-1-yl)-propoxy]-benzoic acid ethyl ester (350 mg, 74%). HPLC-MS 430 [M+1]+.
WORKUP
后处理
- temperaturewas maintained for 54 h
- temperatureAfter this time, the mixture was cooled to rt
- filtrationfiltered
- concentrationThe filtrate was concentrated under reduced pressure
- washwashed with diethyl ether and petroleum ether
- customdried