HRID653536

反应详情

EQUATION

反应方程式

HRID 653536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.3 g (1.91 mmol) of 2,4-dicyano-3-methylaniline, 0.44 g (3.82 mmol) of chloroformamidine hydrochloride, and 0.7 g of dimethylsulfone was heated to 170°-175° C. The mixture solidified after a time, and was allowed to cool to room temperature. Water (20 ml) was added, and the resulting mixture was made basic with 1 molar aqueous sodium hydroxide solution, filtered, and washed with water. The solids were triturated with methanol to yield 0.167 g of 2,4-diamino-5-methyl-6-quinazolinecarbonitrile, mp>270° C. The infrared, mass, and proton magnetic resonance spectra corresponded to those of a known sample of the compound.

WORKUP

后处理

  1. temperaturewas heated to 170°-175° C
  2. filtrationfiltered
  3. washwashed with water
  4. customThe solids were triturated with methanol