HRID1715825

反应详情

EQUATION

反应方程式

HRID 1715825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the mixture of 37 g of 2-amino-5-nitrobenzoic acid in 500 mL of dioxane, under stirring 24.5 mL of diphosgene was added dropwise. The mixture was heated under reflux conditions for 6 hours then it was evaporated to dryness. The residue was suspended in 100 mL of diethyl ether and filtered off to give 41.4 g of the title product as HCl salt, m.p.: 256-259° C. LC-MS: MH+ 209; Ret. time: 5 minutes.

WORKUP

后处理

  1. additionwas added dropwise
  2. temperatureThe mixture was heated under reflux conditions for 6 hours
  3. customit was evaporated to dryness
  4. filtrationfiltered off