HRID1531550

反应详情

EQUATION

反应方程式

HRID 1531550 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2-(3,5-dimethylphenyl)-5-amino-1H-indole (1.16 g in 60 mL dry methylene chloride) at −60 ° C. was added 0.86 mL benzyl chloroformate followed by 1 mL diisopropylethylamine and the mixture warmed slowly to 0° C. After 45 minutes, the reaction was quenched by the addition of saturated aqueous ammonium chloride and the mixture extracted with methylene chloride. The organic portion was washed with brine, dried over sodium sulfate and concentrated in vacuo. Purification by flash chromatography (hexane:methylene chloride:ethyl acetate, 8:8:1; then 7:7:1) gave the title compound (1.68 g).

WORKUP

后处理

  1. customthe reaction was quenched by the addition of saturated aqueous ammonium chloride
  2. extractionthe mixture extracted with methylene chloride
  3. washThe organic portion was washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customPurification by flash chromatography (hexane