HRID1901052

反应详情

EQUATION

反应方程式

HRID 1901052 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-methoxy-2-nitroaniline (15.0 g) and diisopropylamine (16.2 ml) in dichloromethane (300 ml) was added dropwise under ice-cooling a solution of phenylchloroformate (16.8 g) in dichloromethane (30 ml). The reaction solution was stirred at room temperature overnight, washed with water and saturated saline and dried over anhydrous MgSO4. The solvent was distilled off. Crystallization of the residue from hexane gave phenyl 4-methoxy-2-nitrophenylcarbamate (12.6 g, 49.1%) as crystals.

WORKUP

后处理

  1. washwashed with water and saturated saline
  2. dry with materialdried over anhydrous MgSO4
  3. distillationThe solvent was distilled off
  4. customCrystallization of the residue from hexane