反应详情

To a solution of 3-phenylisoxazole-5-amine (420 mg, 2.62 mmol) and pyridine (0.636 ml, 7.87 mmol) in tetrahydrofuran (5 ml) was added 2,2,2-trichloroethyl chloroformate (0.542 ml, 3.93 mmol) with ice-cooling, the mixture was stirred for 30 minutes with ice-cooling, the reaction mixture was poured into ice-water and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to obtain the desired product (750 mg, 85.3%) as a solid.

1. temperaturecooling
2. temperaturecooling
3. extractionthe mixture was extracted with ethyl acetate
4. washThe extract was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure