HRID870499

反应详情

EQUATION

反应方程式

HRID 870499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

A suspension of (2S)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate (1:1) (XI) (13 gm, 0.0404 moles) in methanol (260 ml) was heated under reflux, with stirring, for 3 hour. The resulted suspension was allowed to cool to 35° C. and the resulting suspension filtered under suction. The solid was washed with additional methanol (2×13 ml). The solid was dried under reduced pressure (4 mm Hg), to obtain (2S,5R)-5-[(benzyloxy)amino]-2-cyanopiperidine ethanedioate (XIA) as a white solid, 7.3 gm, yield 56%.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux
  3. filtrationthe resulting suspension filtered under suction
  4. washThe solid was washed with additional methanol (2×13 ml)
  5. customThe solid was dried under reduced pressure (4 mm Hg)