HRID268651

反应详情

EQUATION

反应方程式

HRID 268651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of (5-bromo-7-ethyl-1H-indol-3-yl)-oxo-acetic acid ethyl ester (1.55 g, 4.8 mmol) in tetrahydrofuran at room temperature under nitrogen was dropped a 2.0 M solution of lithium borohydride in tetrahydrofuran. The reaction mixture was heated at 90° C. oil bath for 5 hours. After cooling to room temperature, it was quenched with 5% hydrochloric acid solution until the excess lithium borohydride was destroyed. To the mixture was added saturated sodium bicarbonate solution and extracted with ethyl acetate. Extracts were dried over magnesium sulfate and concentrated under reduced pressure to give the crude product of 2-(5-bromo-7-ethyl-1H-indol-3-yl)-ethanol, which went to the next reaction without further purification.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. customit was quenched with 5% hydrochloric acid solution until the excess lithium borohydride
  3. customwas destroyed
  4. additionTo the mixture was added saturated sodium bicarbonate solution
  5. extractionextracted with ethyl acetate
  6. dry with materialExtracts were dried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure