HRID53241

反应详情

EQUATION

反应方程式

HRID 53241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(3-methyl-1,2,4-oxadiazol-5-yl)benzenamine (1.0 g) in dry dichloromethane (20 ml) was added dropwise to a 0° solution of phosgene (14.1 ml, 20% in toluene) in dry dichloromethane (50 ml) under a nitrogen atmosphere. After addition the reaction mixture was allowed to slowly attain room temperature and stirred for 4 h. Nitrogen, was bubbled through the resulting mixture for 16 h. Dichloromethane was added to the resultant precipitate and the solution was evaporated to give the title compound (1.322 g), max (Nujol) 2800-2500, 1782 (NCO-Cl), 1631 (C=N), 1501 (NH), 769 (aromatic) cm-1.

WORKUP

后处理

  1. additionAfter addition the reaction mixture
  2. customwas allowed to slowly attain room temperature
  3. customNitrogen, was bubbled through the resulting mixture for 16 h
  4. additionDichloromethane was added to the resultant precipitate
  5. customthe solution was evaporated