HRID1095457

反应详情

EQUATION

反应方程式

HRID 1095457 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

A suspension of 168 mmol of lithium aluminium hydride in 300 ml of tetrahydrofuran is cooled to 0-5° C. 80.0 mmol of 1-amino-5-methoxyindane-1-carboxylic acid are added in portions, and the reaction mixture is then heated to reflux for 1 hour. The reaction mixture is cooled to room temperature and quenched with 7.8 ml of water, 36.2 ml of 1M sodium hydroxide solution and a further 21.0 ml of water. The reaction mixture is stirred at room temperature for 30 minutes and then filtered through Hyflo. The filtrate is evaporated. The title compound is obtained as a beige solid which is employed without further purification for the next stage. Rt=2.36 (gradient III).

WORKUP

后处理

  1. temperaturethe reaction mixture is then heated
  2. temperatureto reflux for 1 hour
  3. temperatureThe reaction mixture is cooled to room temperature
  4. customquenched with 7.8 ml of water, 36.2 ml of 1M sodium hydroxide solution
  5. filtrationfiltered through Hyflo
  6. customThe filtrate is evaporated