HRID1524287

反应详情

EQUATION

反应方程式

HRID 1524287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add lithium hydroxide (0.50 g, 12 mmol) to a solution of trans-4-(3-bromo-phenyl)-pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester (0.80 g, 2.08 mmol) in a 1:2:1 mixture of MeOH:tetrahydrofuran:water (8 mL). Stir the mixture at room temperature for 3 h then concentrate under reduced pressure to remove volatile organics. Wash the concentrated aqueous mixture with EtOAc and then acidify to pH 5 using a 0.5 M solution of citric acid. Extract the mixture with EtOAc, dry over anhydrous sodium sulfate, and concentrate under reduced pressure to provide 0.53 g of trans-4-(3-bromo-phenyl)-pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester.

WORKUP

后处理

  1. concentrationthen concentrate under reduced pressure
  2. customto remove volatile organics
  3. washWash the concentrated aqueous mixture with EtOAc
  4. extractionExtract the mixture with EtOAc
  5. dry with materialdry over anhydrous sodium sulfate
  6. concentrationconcentrate under reduced pressure