HRID354432

反应详情

EQUATION

反应方程式

HRID 354432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of N-Boc proline methyl ester (2 .0 g, 8.15 mmol) in CH2Cl2 were added 3 A molecular sieves (2 g) and PDC (4.60 g, 12.2 mmol). The mixture was stirred for 3 days. The mixture was filtered through a Celiete pad and the filtrate was evaporated. The residue was chromatographed on silica gel with CHCl3—MeOH (10:1) as eluent to give methyl 1-(tert-butoxycarbonyl)-4-oxopyrrolidine-2-carboxylate (1.13 g, 57%) as a colorless oil. 1H-NMR (CDCl3) δ1.46-1.48 (m, 9 H), 2.56-2.61 (m, 1 H), 2.88-3.00 (m, 1 H), 3.77 (s, 3 H), 3.82-3.88 (m, 2 H), 4.71-4.83 (m, 1 H).

WORKUP

后处理

  1. filtrationThe mixture was filtered through a Celiete pad
  2. customthe filtrate was evaporated
  3. customThe residue was chromatographed on silica gel with CHCl3—MeOH (10:1) as eluent