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
To a suspension of (2-(difluoromethyl)thiazol-4-yl)methanol (44 mg) and 4-chloro-1-(2-cyclopropyl-1-methyl-1H-benzo[d]imidazol-6-yl)pyridin-2(1H)-one (66.5 mg) in toluene (1 ml) was added potassium tert-butoxide (49.8 mg) at 100° C., and the mixture was stirred at 100° C. under dry atmosphere (CaCl2 tube) for 30 min. The mixture was quenched with water and extracted with EtOAc. The organic layer was separated, washed with water and brine successively, dried over MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/EtOAc then EtOAc/MeOH), followed by recrystallization from EtOH-water to give the title compound (47.7 mg) as an off-white solid.
WORKUP
后处理
- dry with materialunder dry atmosphere (CaCl2 tube) for 30 min
- customThe mixture was quenched with water
- extractionextracted with EtOAc
- customThe organic layer was separated
- washwashed with water and brine successively
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel column chromatography (hexane/EtOAc
- customEtOAc/MeOH), followed by recrystallization from EtOH-water