HRID49743

反应详情

EQUATION

反应方程式

HRID 49743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

1.0 g (4.33 mmol) of p-maleinimidophenylacetic acid were suspended in 25 ml of dichloromethane and diluted with a 2.5-fold excess of oxalic acid dichloride (1.37 g, 945 μl; 10.82 mmol). The reaction mixture was heated to 30-40° C. with the exclusion of moisture and stirred for 15 h. Then the solvent was removed under a vacuum and dried under a high vacuum. Crystallization from toluene yielded a yellow powder (yield: 59%); melting point: 154° C.; Rf-value: 0.29 (acetic ester/hexane 4/1)

WORKUP

后处理

  1. customThen the solvent was removed under a vacuum
  2. customdried under a high vacuum
  3. customCrystallization from toluene