HRID1494840

反应详情

EQUATION

反应方程式

HRID 1494840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.54 g of 2-benzyl-4-nitroisoindoline was dissolved in 10 ml of chloroform, and 1.27 g of sodium carbonate was added to the solution. To the mixture was added dropwise 1.30 g of ethyl chloroformate under ice-cooling while stirring. After the addition, the stirring was continued for 20 hours at room temperature. The insoluble materials were removed by filtration and the filtrate was washed with water, 5% hydrochloric acid, and then with water. The mixture was concentrated and recrystallized from a chloroform-ether mixed solvent to obtain 1.73 g of 2-ethoxycarbonyl-4-nitroisoindoline.

WORKUP

后处理

  1. temperaturecooling
  2. additionAfter the addition
  3. customThe insoluble materials were removed by filtration
  4. washthe filtrate was washed with water, 5% hydrochloric acid
  5. concentrationThe mixture was concentrated
  6. customrecrystallized from a chloroform-ether mixed solvent