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 30 mg (0.06 mmol) of 2,4-dichloro-6-methoxy-N-[2,2,2-trifluoro-1-(1H-indol-3-ylmethyl)ethyl]benzenesulfonamide in 2 mL of dichloromethane was added 1 mL (1 mmol) of 1 M boron tribromide in CH2Cl2. After 1 hour, the reaction was cooled in an ice-water bath and cautiously quenched with 5-10 mL of methanol with stirring. The mixture was warmed to room temperature and the residue was dissolved in ethyl acetate and washed with three 20 mL portions of 1 M aqueous HCl, saturated aqueous sodium bicarbonate solution, and brine. The organic layers was dried over sodium sulfate, decanted, and concentrated in vacuo. The product crystallized upon concentration to afford 4 mg (13%) of the title compound.
WORKUP
后处理
- temperaturethe reaction was cooled in an ice-water bath
- customcautiously quenched with 5-10 mL of methanol
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with three 20 mL portions of 1 M aqueous HCl, saturated aqueous sodium bicarbonate solution, and brine
- dry with materialThe organic layers was dried over sodium sulfate
- customdecanted
- concentrationconcentrated in vacuo
- customThe product crystallized upon concentration