HRID1465022
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
4-Fluoro-3-(trifluoromethyl)benzonitrile (2.0 g, 10.58 mmol) was dissolved in dimethyl acetamide (35 mL), morpholine (2.88 mL, 31.73 mmol) was added thereto, and the mixture was subjected to a reaction at 145° C. for 19 hours. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (50 mL), and the organic layer was washed with an aqueous sodium hydrogen carbonate solution (50 mL). The organic layer was washed with water, dried with sodium sulfate, and the solvent was distilled under reduced pressure. The concentrated mixture was crystallized with ethyl acetate (10 mL) and n-hexane (80 mL) to obtain the title compound as a brown solid (2.1 g).
WORKUP
后处理
- customthe mixture was subjected to a reaction at 145° C. for 19 hours
- washthe organic layer was washed with an aqueous sodium hydrogen carbonate solution (50 mL)
- washThe organic layer was washed with water
- dry with materialdried with sodium sulfate
- distillationthe solvent was distilled under reduced pressure
- customThe concentrated mixture was crystallized with ethyl acetate (10 mL) and n-hexane (80 mL)