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
- 60 °C
PROCEDURE
实验过程
To a solution of N-({3-[(3-bromo-5-chlorophenyl)oxy]-4-chloro-2-fluorophenyl}methyl)-4-chloro-1-({[2-(trimethylsilyl)ethyl]oxy}methyl)-1H-imidazole-5-carboxamide (112 mg, 0.180 mmol) and 1,1′-bis(diphenylphosphino)ferrocenedichloropalladium(II) dichloromethane complex (7.33 mg, 8.98 μmol) in THF (10 ml) was added DIBAL-H (1.0 M solution in DCM) (2.55 mg, 0.018 mmol), followed by diethylzinc (1.0 M solution in heptane) (22.18 mg, 0.180 mmol). The reaction mixture was stirred for one hour at 60° C., cooled to room temperature, diluted with EtOAc and washed with water. The solvent was removed and the crude material (64 mg) was used directly in the next step without purification. LC-MS (ES+) m/z 572 [M+H].
WORKUP
后处理
- temperaturecooled to room temperature
- washwashed with water
- customThe solvent was removed
- customthe crude material (64 mg) was used directly in the next step without purification