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
PROCEDURE
实验过程
To a solution of the compound [122](29.7 mg) in N,N-dimethylformamide (0.8 mL) were added zinc cyanide (4.8 mg), tris(dibenzylideneacetone)dipalladium(0) (3.7 mg) and 2-dicyclohexylphosphino-2,4,6-triisopropylbiphenyl (7.8 mg) at room temperature, and then the reaction mixture was subjected to microwave irradiation at 160° C. for 30 minutes. The reaction mixture was quenched with water, and extracted with ethyl acetate, and then the obtained organic layer was dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by reverse phase preparative liquid chromatography to give the titled compound (13.3 mg) as a white solid.
WORKUP
后处理
- customirradiation at 160° C. for 30 minutes
- customThe reaction mixture was quenched with water
- extractionextracted with ethyl acetate
- dry with materialthe obtained organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationthe filtrate was concentrated under reduced pressure
- customThe obtained residue was purified by reverse phase preparative liquid chromatography