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
- -78 °C
PROCEDURE
实验过程
To a cooled (−78° C.) stirred solution of methyl 2-(4-(4-chloro-2-methoxyphenyl)-6-methyl-2-phenylpyrimidin-5-yl)pentanoate (0.125 mg; 0.294 mmol) in dichloromethane (1.5 mL) was added a solution of boron tribromide (1M in dichloromethane) (0.340 mL; 0.340 mmol) dropwise. After 1 h the mixture was allowed to warm up to room temperature and the reaction was stirred for 16 h. The reaction was quenched by adding water and the mixture was extracted with ethyl acetate, dried over magnesium sulphate, filtered and concentrated under reduced pressure. Purifications by flash-chromatography on silica gel using a gradient of methanol (0-10%) in dichloromethane and by preparative TLC on silica gel using a mixture methanol-dichloromethane (5:95) as eluent furnished 0.0018 g (1.5%) of the title compound.
WORKUP
后处理
- temperatureto warm up to room temperature
- customThe reaction was quenched
- additionby adding water
- extractionthe mixture was extracted with ethyl acetate
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure