HRID1197408

反应详情

EQUATION

反应方程式

HRID 1197408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

While stirring and within a period of 1 1/2 hours at 0° to 5° C., 293.1 g (1.692 mol) of a 30% strength sodium methylate solution was added to a solution of 434 g (1.692 mol) of 2,6-dichloro-4-trichloromethylpyrimidine in 1 liter of 1,2-dichloroethane. The mixture was stirred for 1 hour at 0° to 5° C. and for 12 hours at 25° C. The reaction mixture was then extracted with water and saturated sodium chloride solution. After drying over magnesium sulfate and evaporating down, there was obtained 423 g (95% of theory) of the title compound as an almost colorless oil of nD23 =1.5552. 1H-NMR (CDCl3) (ppm) OCH3 (s/3H) 4.1; CH (s/1H) 7.25.

WORKUP

后处理

  1. stirringThe mixture was stirred for 1 hour at 0° to 5° C. and for 12 hours at 25° C
  2. extractionThe reaction mixture was then extracted with water and saturated sodium chloride solution
  3. dry with materialAfter drying over magnesium sulfate
  4. customevaporating down