HRID1986190

反应详情

EQUATION

反应方程式

HRID 1986190 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

Benzo[b]thiophene-6-carbonitrile (9.70 g, 61.1 mmol) is dissolved in THF (400 mL) and cooled to 0-5° C. Lithium aluminum hydride (183 mL of 1.0 M solution in THF) is added dropwise over 30 minutes and the reaction is stirred for 20 hours while warming to 25° C. The reaction is cooled with an ice bath and water (6.94 mL) is slowly added followed by 15% sodium hydroxide (6.94 mL) and water (20.83 mL). The resulting precipitate is filtered and washed with diethyl ether. The filtrate is concentrated to give the title compound as a colorless oil (8.16 g, 82% yield). ES+(m/z) 164 [M+H].

WORKUP

后处理

  1. temperaturewhile warming to 25° C
  2. temperatureThe reaction is cooled with an ice bath
  3. filtrationThe resulting precipitate is filtered
  4. washwashed with diethyl ether
  5. concentrationThe filtrate is concentrated