HRID1662083

反应详情

EQUATION

反应方程式

HRID 1662083 的结构方程式

PROCEDURE

实验过程

An autoclave was cooled with an acetone/dry ice bath, and an ammonia gas was blown to pool 477 cc of liquid ammonia (corresponding to 25 equivalent of (S)-1-benzyl-3-(methanesulfonyloxy)pyrrolidine). Thereto was added 180 g of (S)-1-benzyl-3-(methanesulfonyloxy)pyrrolidine (672.1 mmol, optical purity: 100% e.e.), which was heated to 100° C. whereby an internal pressure of 55 barr was observed. After allowing the reaction for 5 hrs, the reaction mixture was cooled to room temperature, and ammonia was removed by distillation under reduced pressure. As the residue, 306.7 g of a brown oily material was obtained (reaction yield: 88%, optical purity: 91.2% e.e.).

WORKUP

后处理

  1. temperatureAn autoclave was cooled with an acetone/dry ice bath
  2. customthe reaction for 5 hrs
  3. customammonia was removed by distillation under reduced pressure