HRID1442971

反应详情

EQUATION

反应方程式

HRID 1442971 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the (2S,4S)-4-(3-chloro-phenylamino)-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (200 mg, 0.58 mmol) in THF (2 ml) was added a solution of LiOH.H2O (73 mg 1.74 mmol), and the reaction stirred at room temperature overnight. The solvent was concentrated in vacuo and the residual aqueous solution washed with DCM (2 ml). The aqueous was then adjusted to pH 5 with saturated aqueous citric acid and re-extracted with DCM (2×10 ml). These combined extracts were dried over MgSO4 and evaporated to give the title compound as a white foam (168 mg, 88%)

WORKUP

后处理

  1. concentrationThe solvent was concentrated in vacuo
  2. washthe residual aqueous solution washed with DCM (2 ml)
  3. extractionre-extracted with DCM (2×10 ml)
  4. dry with materialThese combined extracts were dried over MgSO4
  5. customevaporated