HRID2240919

反应详情

EQUATION

反应方程式

HRID 2240919 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.7 g (0.03 mol) of sodium methylate are added to a solution of 3.45 g (0.03 mol) of N-hydroxy succinimide in 25 ml of methanol. The reaction mixture is stirred for one h, concentrated under vacuo and the residue is taken up in 15 ml of DMF. 4.6 g (0.03 mol) of methyl benzimidoyl chloride are added on stirring. The reaction mixture is stirred at room temperature for 12 h and then poured into 120 ml of water. The so formed precipitate is sucked off and dried in vacuo to obtain 3.8 g of a crude product which is then taken up and recrystallised in 9 ml of toluene to give 3.05 g of N-methyl-benzimidic acid 2,5-dioxopyrrolidine-1-yl ester in form of colorless crystals; mp. 119-120° C.

WORKUP

后处理

  1. concentrationconcentrated under vacuo
  2. stirringon stirring
  3. stirringThe reaction mixture is stirred at room temperature for 12 h
  4. customThe so formed precipitate
  5. customdried in vacuo
  6. customto obtain 3.8 g of a crude product which
  7. customrecrystallised in 9 ml of toluene