HRID1760083

反应详情

EQUATION

反应方程式

HRID 1760083 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a THF solution of (S)-3-phenyl-3-hydroxypropanenitrile was slowly added THF solution of borane dimethyl sulfide complex at room temperature. Methyl sulfide was then distilled from the reaction vessel and the resulting THF solution refluxed for 2.5 h. After cooling to room temperature methanolic HCl was added to the reaction mixture. Methanol and methyl borate were removed by distillation and the reaction mixture neutralized with sodium hydroxide (5N). Extraction of the mixture with dichloromethane,followed by concentration provided the crystalline (S)-3-phenyl-3-hydroxypropylamine.

WORKUP

后处理

  1. customat room temperature
  2. distillationMethyl sulfide was then distilled from the reaction vessel
  3. temperaturethe resulting THF solution refluxed for 2.5 h
  4. additionwas added to the reaction mixture
  5. customMethanol and methyl borate were removed by distillation
  6. extractionExtraction of the mixture with dichloromethane,followed
  7. concentrationby concentration