HRID1158344

反应详情

EQUATION

反应方程式

HRID 1158344 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of (3S*,4S*)-1-benzyl-pyrrolidine-3,4-dicarboxylic acid diethyl ester (82.8 g, 271.14 mmol), di-tert-butylcarbonate (88.76 g, 406.71 mmol) and Pd/C 10% (8 g) in EtOH (1.5 L) is stirred under hydrogen atmosphere. The crude material is filtered over a pad of Celite and concentrated. The crude material is purified by flash chromatography on silica gel (eluent: CH2Cl2/acetone 100:0 to 95:5). TLC, Rf (CH2Cl2/acetone 95:5)=0.51. MS (LC-MS): 216.2 [M+H-Boc]+.

WORKUP

后处理

  1. filtrationThe crude material is filtered over a pad of Celite
  2. concentrationconcentrated
  3. customThe crude material is purified by flash chromatography on silica gel (eluent: CH2Cl2/acetone 100:0 to 95:5)