反应详情

A solution of 3,5-bis(trifluoromethyl)benzothioamide (1) (205.65 g) in DMF (1.03 L) was treated with hydrazine hydrate (73.16 mL, 2.0 eq). The reaction mixture was stirred at ambient temperature for 1 h. before being treated with formic acid (1.03 L). The reaction mixture was refluxed at 90° C. for 2-3 h then allowed to cool down to ambient temperature, poured into saturated aqueous sodium bicarbonate (7 L) and extracted with EtOAc (3×1 L), The combined organic layers were washed with brine (3×500 mL), dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure to afford 180 g of crude compound. This crude material was washed with petroleum ether (3×500 mL), filtered and dried well to afford 160 grams (75% yield) of triazole (2) obtained as a pale yellow solid.

1. temperatureThe reaction mixture was refluxed at 90° C. for 2-3 h
2. temperatureto cool down to ambient temperature
3. extractionextracted with EtOAc (3×1 L)
4. washThe combined organic layers were washed with brine (3×500 mL)
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customto afford 180 g of crude compound
9. washThis crude material was washed with petroleum ether (3×500 mL)
10. filtrationfiltered
11. customdried well