HRID1719787
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
PROCEDURE
实验过程
30 ml of a 40% aqueous methylamine solution are added, at a temperature of between 20° and 25° C., to 2.2 g (0.009 mol) of 2-methylsulfonyl-4-difluoromethoxy-6-methylpyrimidine. The mixture warms up to a temperature of 60° C. The reaction mixture is subsequently stirred for half an hour at the same temperature; it is then cooled and 50 ml of methylene chloride are added. The organic phase is separated, dried over sodium sulfate and concentrated by evaporation. Crystallisation of the residue from a methylene chloride/petroleum ether mixture yields 1.4 g (74% of theory) of 2-methylamino-4-difluoromethoxy-6 -methylpyrimidine, m.p. 129.5°-131° C.
WORKUP
后处理
- customwarms up to a temperature of 60° C
- temperatureit is then cooled
- customThe organic phase is separated
- dry with materialdried over sodium sulfate
- concentrationconcentrated by evaporation
- customCrystallisation of the residue from a methylene chloride/petroleum ether mixture