HRID1352100

反应详情

EQUATION

反应方程式

HRID 1352100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-(azidomethyl)-2-chlorobenzoic acid (6.82 g, 32.2 mmol), N-hydroxysuccinimide (5.19 g, 45.1 mmol) and dicyclohexylcarbodiimide (9.31 g, 45.1 mmol) in tetrahydrofuran (250 Ml) was stirred overnight at room temperature. The dicyclohexylurea (7.70 g, 76%) was filtered off and discarded. Silica gel was added, the solvent was evaporated and the residue was chromatographed (40–60% ethyl acetate/hexanes) to give 1-[[4-(azidomethyl)-2-chlorobenzoyl]oxy]-2,5-pyrrolidinedione (9.64 g, 97%) as a white solid.

WORKUP

后处理

  1. filtrationThe dicyclohexylurea (7.70 g, 76%) was filtered off
  2. additionSilica gel was added
  3. customthe solvent was evaporated
  4. customthe residue was chromatographed (40–60% ethyl acetate/hexanes)