反应详情

A slurry of 18 g (0.45 mole) of lithium aluminum hydride in 1000 mL of dry tetrahydrofuran was cooled to 5° C. while stirring under nitrogen. To the slurry was added alpha-(2-(4-chlorophenyl)ethyl)-alpha-phenyl-1H-1,2,4-triazole-1-propanenitrile in 2000 mL of dry., tetrahydrofuran over 3 hours. The reaction was kept at 5°-10° C. during the addition then allowed to warm to room temperature and stirred overnight. The reaction was cooled in an ice bath and quenched with the slow addition of sodium sulfate. The solvent was removed and the residue was extracted with ethyl acetate and washed with 1000 mL water and 1000 mL brine. After drying, and removal of the solvent, 137 g (89.5% yield) of a very viscous oil resulted.

1. customof dry
2. additionThe reaction was kept at 5°-10° C. during the addition
3. stirringstirred overnight
4. temperatureThe reaction was cooled in an ice bath
5. customquenched with the slow addition of sodium sulfate
6. customThe solvent was removed
7. extractionthe residue was extracted with ethyl acetate
8. washwashed with 1000 mL water and 1000 mL brine
9. customAfter drying
10. customremoval of the solvent, 137 g (89.5% yield) of a very viscous oil
11. customresulted