HRID1262694

反应详情

EQUATION

反应方程式

HRID 1262694 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a magnetically stirred suspension of 9.7 g. (40 mmol) of 1-(2',6'-dimethylphenyl)amidinourea hydrochloride in 50 ml. of CH3CN at room temperature is added 5.7 g. (48 mmol) of N,N-dimethylformamide dimethylacetal. The reaction mixture is stirred for 10 minutes after which all of the solid material goes into solution. The solution is stirred for 5 minutes after which a seed crystal is added. A white solid precipitates. The reaction mixture is stirred for an additional 1.5 hours, after which the solid precipitate is filtered to yield 1-(2',6'-dimethylphenyl)-4-amino-1,2-dihydro-1,3,5-triazin-2-one, melting point 248.5°-249.5° C. When recrystallized from absolute EtOH the product is obtained as a white solid with melting point 258.6°-259° C.

WORKUP

后处理

  1. additionTo a magnetically stirred suspension of 9.7 g
  2. stirringThe solution is stirred for 5 minutes after which a seed crystal
  3. additionis added
  4. customA white solid precipitates
  5. stirringThe reaction mixture is stirred for an additional 1.5 hours
  6. filtrationafter which the solid precipitate is filtered