HRID81585

反应详情

EQUATION

反应方程式

HRID 81585 的结构方程式

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

  1. customThe sealed reaction vessel
  2. customwas lowered to 70° C.
  3. customThe reaction mixture was evaporated
  4. custompurified on a silica gel column
  5. washby eluting with CH2Cl2/1-4% EtOH:NH3 9:1