HRID1163351

反应详情

EQUATION

反应方程式

HRID 1163351 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of 2.9 (3R,4R) and (3S,4S)-1-benzyl-4-(tert-butoxycarbonylamino-methyl)-pyrrolidine-3-carboxylic acid ethyl ester (8.0 mmol) in 50 ml THF were added 671 mg lithium hydroxide mono hydrate (16 mmol) and 0.5 ml water. The solution was stirred at 40° C. and the reaction monitored by TLC. After 72 h the solvent was evaporated, the residue dissolved in dichloromethane, washed with water and brine, dried over Mg sulfate, filtered and evaporated. The residue was crystallized from a dichloromethane/hexane mixture.

WORKUP

后处理

  1. customAfter 72 h the solvent was evaporated
  2. dissolutionthe residue dissolved in dichloromethane
  3. washwashed with water and brine
  4. dry with materialdried over Mg sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was crystallized from a dichloromethane/hexane mixture