HRID2202897
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
A mixture of 4-((4-chlorobenzyl)oxy)pyridin-2(1H)-one (100 mg), 6-bromo-2-(2,2-difluorocyclopropyl)-1-methyl-1H-benzimidazole (122 mg), potassium carbonate (176 mg), N,N′-dimethylethylenediamine (0.046 ml), copper iodide (81 mg) and DMSO (3 ml) was stirred at 150° C. under Ar atmosphere for 1 h. The mixture was quenched with 28% NH3 solution and the precipitate was collected by filtration. The solid was dissolved in THF, passed through NH silica gel pad and concentrated in vacuo. The precipitate was recrystallized from EtOAc/MeOH to give the title compound (2 mg) as a pale orange solid.
WORKUP
后处理
- customThe mixture was quenched with 28% NH3 solution
- filtrationthe precipitate was collected by filtration
- dissolutionThe solid was dissolved in THF
- concentrationconcentrated in vacuo
- customThe precipitate was recrystallized from EtOAc/MeOH