HRID2217844
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
- 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
- temperaturewas cooled to room temperature
- concentrationconcentrated
- customPurification (SiO2, dichloromethane:methanol:ammonia in methanol (7 M) 95:5:0.5), conversion to the dihydrochloride salt by treatment
- customwith hydrochloric acid (4M in 1,4-dioxane) and recrystallisation (methanol/ethyl acetate)