HRID1901058

反应详情

EQUATION

反应方程式

HRID 1901058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-fluoro-2-nitroaniline (1.56 g) and diisopropylamine (1.68 ml) in dichloromethane (20 ml) was added dropwise under ice-cooling phenyl chloroformate (1.51 g). After stirring the mixture at room temperature overnight, the reaction solution was washed with water, saturated saline, dried over anhydrous MgSO4 and the solvent was distilled off. Crystallization of the residue from diisopropyl ether afforded phenyl 4-fluoro-2-nitrophenylcarbamate (0.79 g, 29%) as crystals.

WORKUP

后处理

  1. washthe reaction solution was washed with water, saturated saline
  2. dry with materialdried over anhydrous MgSO4
  3. distillationthe solvent was distilled off
  4. customCrystallization of the residue from diisopropyl ether