反应详情

To a solution of 1,2,3-thiadiazol-5-amine and pyridine (0.129 ml, 4.00 mmol) in tetrahydrofuran (4.5 ml) was added 2,2,2-trichloroethyl chloroformate (0.220 ml, 2.00 mmol) under ice-cooling, and the mixture was stirred at room temperature for 2 hours. Water was poured to the reaction mixture, 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. Hexane was added to the residue, and 190 mg (51.6%) of the desired product was collected by filtration as a solid.

1. temperaturecooling
2. extractionthe mixture was extracted with ethyl acetate
3. washThe extract was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. additionHexane was added to the residue, and 190 mg (51.6%) of the desired product
7. filtrationwas collected by filtration as a solid