HRID2217844

反应详情

EQUATION

反应方程式

HRID 2217844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A stirred suspension of 2,6-dichloro-N-(cyclohexylmethyl)quinoline-5-carboxamide (Example 43 (a)) (200 mg) and N,N′-dimethyl-1,2-ethanediamine (0.30 mL) in acetonitrile (2 mL) was heated at 100° C. in a microwave for 90 minutes after which it was cooled to room temperature and concentrated. Purification (SiO2, dichloromethane:methanol:ammonia in methanol (7 M) 95:5:0.5), conversion to the dihydrochloride salt by treatment with hydrochloric acid (4M in 1,4-dioxane) and recrystallisation (methanol/ethyl acetate) afforded the title compound as a solid (160 mg).

WORKUP

后处理

  1. temperaturewas cooled to room temperature
  2. concentrationconcentrated
  3. customPurification (SiO2, dichloromethane:methanol:ammonia in methanol (7 M) 95:5:0.5), conversion to the dihydrochloride salt by treatment
  4. customwith hydrochloric acid (4M in 1,4-dioxane) and recrystallisation (methanol/ethyl acetate)