反应详情

温度

50 °C

Combine 1-benzyl-4-phenyl-4-cyanopiperidine (535 g, 1940 mmol), aqueous sodium hydroxide (85 mL, 50% by weight), and ethanol (5 L). Heat to 50° C. Remove the heating and add a solution of hydrogen peroxide (856 mL, 30% by weight in water) at such a rate that the temperature of the reaction mixture does not rise above 50° C. After the addition of hydrogen peroxide is complete, maintain the temperature of reaction mixture at 50° C. After 20 hours, dilute the reaction mixture with water (3 L) and concentrate invacuo at 35° C. to remove the ethanol. Cool the reaction mixture to ambient temperature to give a solid. Collect the solid by filtration, rinse with water, and air dried to give 1-benzyl-4-phenylpiperidine-4-carboxylic acid amide N-oxide.

1. customRemove the heating and
2. additionadd a solution of hydrogen peroxide (856 mL, 30% by weight in water) at such a rate that the temperature of the reaction mixture
3. customdoes not rise above 50° C
4. additionAfter the addition of hydrogen peroxide
5. temperaturemaintain
6. customthe temperature of reaction mixture at 50° C
7. concentrationconcentrate invacuo at 35° C.
8. customto remove the ethanol
9. temperatureCool the reaction mixture to ambient temperature
10. customto give a solid
11. customCollect the solid
12. filtrationby filtration
13. washrinse with water, and air
14. customdried