HRID1524286

反应详情

EQUATION

反应方程式

HRID 1524286 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Add a saturated aqueous solution of sodium bicarbonate (350 mL) to a solution of trans-4-(3-bromo-phenyl)-pyrrolidine-3-carboxylic acid methyl ester (11 g, 38 mmol) in methylene chloride (350 mL). Cool the mixture to 0° C. and add BOC-anhydride (8.9 g, 41 mmol) dropwise. Slowly warm the mixture to room temperature and stir for 12 h. Extract the reaction mixture with methylene chloride, dry the combined organic phase over anhydrous sodium sulfate and concentrate under reduced pressure. Purify the residue by silica gel chromatography to provide 13 g of trans-4-(3-bromo-phenyl)-pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester 3-methyl ester.

WORKUP

后处理

  1. temperatureSlowly warm the mixture to room temperature
  2. extractionExtract the reaction mixture with methylene chloride
  3. dry with materialdry the combined organic phase over anhydrous sodium sulfate
  4. concentrationconcentrate under reduced pressure
  5. customPurify the residue by silica gel chromatography