反应 #740718

ord-aa481005c3ed4f19bc72491e7818d2d7

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated to 170°-175° C
  2. 2
    过滤filtered
  3. 3
    洗涤washed with water
  4. 4
    其他The solids were triturated with methanol

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04677219uspto-grants-1987_06