HRID2082259
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringStirring
- customThe reaction mixture was evaporated down under reduced pressure
- washthe residue was washed with water
- customdried
- washThe reaction product was then washed onto a silica gel column with methylene chloride
- washeluted with the same solvent