HRID81585
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
5-Difluoromethyl-5-(2-fluoro-phenyl)-2,2-dimethyl-morpholine-3-thione (2.50 g, 8.64 mmol) was dissolved in NH3 solution 7 mol/L in methanol (40.7 mL, 285 mmol). The sealed reaction vessel was heated to 80° C. for 7 h, then the temperature was lowered to 70° C. and the reaction mixture was stirred over night. The reaction mixture was evaporated and purified on a silica gel column by eluting with CH2Cl2/1-4% EtOH:NH3 9:1 to give 2.09 g of the title compound as an off-white solid.
WORKUP
后处理
- customThe sealed reaction vessel
- customwas lowered to 70° C.
- customThe reaction mixture was evaporated
- custompurified on a silica gel column
- washby eluting with CH2Cl2/1-4% EtOH:NH3 9:1