反应详情

温度

50 °C

A mixture of 5-benzhydrylthio-2-(2-propynyl)-2H-tetrazole (1.05 g), anisole (1.79 g) and trifluoroacetic acid (9.7 ml) was stirred at 22° C. for 1.5 hours, at 35° C. for an hour, at 50° C. for 1.7 hours and then at room temperature for a further 14 hours. The reaction mixture was filtered and the filtrate was evaporated under reduced pressure. To the residue was added a saturated aqueous solution of sodium bicarbonate (10 ml) and the mixture was adjusted to pH 8.5 with 2 N aqueous solution of sodium hydroxide. The aqueous layer was separated, washed with ethyl acetate (20 ml×2) and thereto was added ethyl acetate. The resulting mixture was adjusted to pH 2.5 with 10% hydrochloric acid. The ethyl acetate layer was separated, washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate and then evaporated to give an oil of 2-(2-propynyl)-2H-tetrazole-5-thiol (0.3 g).

1. waitat room temperature for a further 14 hours
2. filtrationThe reaction mixture was filtered
3. customthe filtrate was evaporated under reduced pressure
4. additionTo the residue was added a saturated aqueous solution of sodium bicarbonate (10 ml)
5. customThe aqueous layer was separated
6. washwashed with ethyl acetate (20 ml×2)
7. additionwas added ethyl acetate
8. customThe ethyl acetate layer was separated
9. washwashed with a saturated aqueous solution of sodium chloride
10. dry with materialdried over magnesium sulfate
11. customevaporated