反应详情

To 21 g (0.55 mole) of lithium aluminum hydride was charged 127 g (0.50 mole) alpha-butyl-alpha-phenyl-1H-1,2,4-triazole-1-propanenitrile in 2500 mL of dry ether over 2.5 hours with stirring under nitrogen. The reaction was stirred for an additional 5 hours after which GLC indicated the reaction was complete. The reaction was quenched with sodium sulfate, filtered and the organic phase separated. The aqueous phase was extracted with 1000mL of ether. The organics were combined, washed with 3×1.5 liters of ice water, dried, filtered and concentrated without external heating and gave 88 g (69.2% yield) of a pale green oil.

1. stirringThe reaction was stirred for an additional 5 hours after which GLC
2. customThe reaction was quenched with sodium sulfate
3. filtrationfiltered
4. customthe organic phase separated
5. extractionThe aqueous phase was extracted with 1000mL of ether
6. washwashed with 3×1.5 liters of ice water
7. customdried
8. filtrationfiltered
9. concentrationconcentrated
10. temperaturewithout external heating