反应详情

温度

80 °C

A mixture of 150 mg of 10% palladium-on-carbon and 400 mg of 2-{4-[4-nitro-3-(propan-2-yloxy)phenyl]-3,6-dihydropyridin-1(2H)-yl}ethanol in 15 ml of ethanol is heated at 80° C. with stirring. 1.25 g of ammonium formate are then added in two portions. After stirring at 80° C. for 1 h, the mixture is allowed to return to ambient temperature and is filtered on Clarcel. The Clarcel is rinsed with 200 ml of ethanol and the filtrate is concentrated under vacuum, so as to obtain a residue which is solubilised in 150 ml of dichloromethane. The organic phase is washed three times with 70 ml of a saturated potassium carbonate solution, and the aqueous phase is extracted twice with 100 ml of dichloromethane. The combined organic phases are dried over magnesium sulfate, filtered and concentrated under vacuum, so as to obtain 330 mg of 2-{4-[4-amino-3-(propan-2-yloxy)phenyl]piperidin-1-yl}ethanol used without further purification.

1. stirringAfter stirring at 80° C. for 1 h
2. customto return to ambient temperature
3. filtrationis filtered on Clarcel
4. washThe Clarcel is rinsed with 200 ml of ethanol
5. concentrationthe filtrate is concentrated under vacuum
6. customso as to obtain a residue which
7. washThe organic phase is washed three times with 70 ml of a saturated potassium carbonate solution
8. extractionthe aqueous phase is extracted twice with 100 ml of dichloromethane
9. dry with materialThe combined organic phases are dried over magnesium sulfate
10. filtrationfiltered
11. concentrationconcentrated under vacuum