HRID2082259

反应详情

EQUATION

反应方程式

HRID 2082259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

7.8 g (0.46 mol) of ammonia were passed into a mixture of 50.0 g (0.23 mol) of 2,4-difluoro-6-chlorodifluoromethoxy-1,3,5-triazine in 150 ml of tetrahydrofuran in the course of 45 minutes at -70° C., while stirring. Stirring was continued for 2 hours at -70° C. and overnight while warming up to 22° C. The reaction mixture was evaporated down under reduced pressure and the residue was washed with water and dried. The reaction product was then washed onto a silica gel column with methylene chloride and eluted with the same solvent. 21.5 g (43.6% of theory) of 2-amino-4-fluoro-6-chlorodifluoromethoxy-1,3,5-triazine of melting point 131°-133° C. were obtained in fractions 1 to 8.

WORKUP

后处理

  1. stirringStirring
  2. customThe reaction mixture was evaporated down under reduced pressure
  3. washthe residue was washed with water
  4. customdried
  5. washThe reaction product was then washed onto a silica gel column with methylene chloride
  6. washeluted with the same solvent