反应详情

温度

5 °C

To a 5 liter flask stirring under nitrogen, fitted with a mechanical stirrer, was charged 18 g (0.45 mole) of lithium aluminum hydride in 1000 mL of dry tetrahydrofuran which was then cooled to 5° C. To the slurry was added 152 g (0.45 mole) of 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. customfitted with a mechanical stirrer
2. additionThe reaction was kept at 5°-10° C. during the addition
3. temperatureto warm to room temperature
4. stirringstirred overnight
5. temperatureThe reaction was cooled in an ice bath
6. customquenched with the slow addition of sodium sulfate
7. customThe solvent was removed
8. extractionthe residue was extracted with ethyl acetate
9. washwashed with 1000 mL water and 1000 mL brine
10. customAfter drying
11. customremoval of the solvent, 137 g (89.5% yield) of a very viscous oil
12. customresulted