反应详情

温度

100 °C

To a 500 mL flask was charged 100.0 g (0.38 mole) of alpha-(4-chlorophenyl)-alpha-ethyl-1H-1,2,4-triazole-1-propanenitrile and 100 mL of dimethyl sulfoxide. To the stirring solution was added 100 g (1.25 mole) of 50% sodium hydroxide. The reaction mixture was heated at 100° C. for 1 hour after which GLC indicated the starting material was consumed. The reaction was poured into water and extracted with ethyl acetate. After washing with brine, the organic phase was dried over magnesium sulfate and concentrated under vacuum without heating. Removal of the solvent gave a foamy glassy solid which was triturated with hexane, filtered and gave 97 g (91% yield) of a white solid, melting point 139°-140° C.

1. customwas consumed
2. additionThe reaction was poured into water
3. extractionextracted with ethyl acetate
4. washAfter washing with brine
5. dry with materialthe organic phase was dried over magnesium sulfate
6. concentrationconcentrated under vacuum
7. temperaturewithout heating
8. customRemoval of the solvent
9. customgave a foamy glassy solid which
10. customwas triturated with hexane
11. filtrationfiltered