HRID1868426

反应详情

EQUATION

反应方程式

HRID 1868426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe reaction was cooled in an ice-water bath
  2. customcautiously quenched with 5-10 mL of methanol
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washwashed with three 20 mL portions of 1 M aqueous HCl, saturated aqueous sodium bicarbonate solution, and brine
  5. dry with materialThe organic layers was dried over sodium sulfate
  6. customdecanted
  7. concentrationconcentrated in vacuo
  8. customThe product crystallized upon concentration