HRID265981

反应详情

EQUATION

反应方程式

HRID 265981 的结构方程式

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

4-Phenyl-4-cyano-1-benzyl-piperidine (535 g, 1940 mmol) was combined with aqueous sodium hydroxide (85 mL, 50% by weight) and ethanol (5 L) and the mixture was heated to 50° C. The heating was removed, and a solution of hydrogen peroxide (856 mL, 30% by weight in water) was added at such a rate that the temperature of the reaction mixture does not rise above 50° C. The reaction mixture was then stirred at 50° C. for 20 hours. The reaction mixture was diluted with water (3 L) and the ethanol was removed in vacuo at 35° C. Cooling the reaction mixture to ambient temperature gave a solid which was collected by filtration, rinsed with water, and air dried to give 4-phenyl-1-benzyl-piperidine-4-carboxylic acid amide N-oxide.

WORKUP

后处理

  1. customThe heating was removed
  2. additiona solution of hydrogen peroxide (856 mL, 30% by weight in water) was added at such a rate that the temperature of the reaction mixture
  3. customdoes not rise above 50° C
  4. additionThe reaction mixture was diluted with water (3 L)
  5. customthe ethanol was removed in vacuo at 35° C
  6. temperatureCooling the reaction mixture to ambient temperature
  7. customgave a solid which
  8. filtrationwas collected by filtration
  9. washrinsed with water, and air
  10. customdried