Ethanol → (1-Benzyl-4-phenylpiperidine-4-carbonyl)-oxidoazanium

HRID 343499

반응식

HRID 343499 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)([C:14]#[N:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-:22].[Na+].C([OH:26])C>O>[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)([C:14]([NH2:15]=[O:26])=[O:22])[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 1914081-Benzyl-4-cyano-4-phenylpiperidine

생성물 1

HCID 88146759(1-Benzyl-4-phenylpiperidine-4-carbonyl)-oxidoazanium

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0da2ce208f80494cb708abb7faf67f4b
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05861417

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