4-Piperidone → 1-[(2,6-Dimethylphenyl)aminocarbonylmethyl]-4-piperidone

HRID 615378노트

반응식

HRID 615378 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][C:10]([CH2:12]Cl)=[O:11].[NH:14]1[CH2:19][CH2:18][C:17](=[O:20])[CH2:16][CH2:15]1>C(O)C>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][C:10]([CH2:12][N:14]1[CH2:19][CH2:18][C:17](=[O:20])[CH2:16][CH2:15]1)=[O:11]

참가 물질

4

반응물 2

HCID 337214-PiperidoneHCID 707982-Chloro-N-(2,6-dimethylphenyl)acetamide

생성물 1

HCID 133933531-[(2,6-Dimethylphenyl)aminocarbonylmethyl]-4-piperidone

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The crude [(2,6-dimethylphenyl)aminocarbonylmethyl]chloride, prepared in Preparation B (50 g., 0.25 moles) and 4-piperidone (86 g, 1 mole) are dissolved in 500 ml of ethanol. The mixture is refluxed for two hours, and then cooled and evaporated. The product is recovered by adding aqueous ammonia to the residue, and extracting with methylene chloride. Three portions of methylene chloride are used, which are collected, washed with water, and evaporated to a semi-solid. Upon addition of diethylether, the product crystallizes and is filtered. The resulting crude mixture is boiled with ether and then evaporated to a residue and triturated with hexane to yield pure material, 1-[(2,6-dimethylphenyl)aminocarbonylmethyl]-4-piperidone. This material is of sufficient purity for use in Reaction Sequences 2 to 5.

후처리

  1. temperatureThe mixture is refluxed for two hours
  2. temperaturecooled
  3. customevaporated
  4. customThe product is recovered
  5. additionby adding aqueous ammonia to the residue
  6. extractionextracting with methylene chloride
  7. customwhich are collected
  8. washwashed with water
  9. customevaporated to a semi-solid
  10. additionUpon addition of diethylether
  11. customthe product crystallizes
  12. filtrationis filtered
  13. customevaporated to a residue
  14. customtriturated with hexane

출처 및 근거

ORD 기록
ord-0839b93d1c3545e9a57da228cce56959
출처 데이터셋
uspto-grants-1985_02
특허 번호
US04499100

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