HRID1859011
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
- 0 °C
PROCEDURE
实验过程
To a mixture of compound 2 (674 mg, 2 mmol) and triethylamine (0.55 ml, 4 mmol) in tetrahydrofuran (10 ml) was added dropwise 2,4-difluorobezoyl chloride (440 mg, 2.5 mmol) in 5 ml tetrahydrofuran at 0° C. The reaction mixture was stirred at 0° C. for 30 minutes and at room temperature for 18 h. The solvent was removed under reduced pressure, the residue was dissolved in dichloromethane (50 ml). The organic phase was washed with brine, dried over sodium sulphate. The solvent was removed under reduced pressure and the resulting product was purified on a column of silica gel (EtOAc/hexane, 9:1) to give the title compound as colorless prisms (448 mg, 47%).
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- dissolutionthe residue was dissolved in dichloromethane (50 ml)
- washThe organic phase was washed with brine
- dry with materialdried over sodium sulphate
- customThe solvent was removed under reduced pressure
- customthe resulting product was purified on a column of silica gel (EtOAc/hexane, 9:1)