反应详情

温度

25 °C

Ammonium acetate (700 g, 9.09 mol) was added to a stirred solution of 1-t-butyloxy carbonyl-3,3-dimethyl-4-piperidone (352 g, 1.55 mol) in methanol (1.0 L). The suspension was stirred for 3 hr at 20-30° C. The reaction mixture was cooled to 0° C. and sodiumcyanoborohydride (45 g, 0.71 mol) was added portion wise over 30 minutes. Cooling was removed and the suspension was stirred for 12 hr at 20-30° C. The reaction mixture was concentrated to dryness, stirred with water (2.0 L) and extracted with 1.0 L×3 dichloromethane. Combined organic extract was washed with water and dried over sodium sulfate. Evaporation of organic solvent afforded the product.

1. temperatureThe reaction mixture was cooled to 0° C.
2. temperatureCooling
3. customwas removed
4. stirringthe suspension was stirred for 12 hr at 20-30° C
5. concentrationThe reaction mixture was concentrated to dryness
6. stirringstirred with water (2.0 L)
7. extractionextracted with 1.0 L×3 dichloromethane
8. extractionCombined organic extract
9. washwas washed with water
10. dry with materialdried over sodium sulfate
11. customEvaporation of organic solvent
12. customafforded the product