Hydrochloric Acid → 2-(p-Methoxybenzyl)-1,3,3-trimethyl-4-piperidone hydrochloride

HRID 596867노트

반응식

HRID 596867 반응식
[CH3:1][O:2][C:3]1[CH:23]=[CH:22][C:6]([CH2:7][CH:8]2[C:13]([CH3:15])([CH3:14])[C:12](=[O:16])[CH:11](C(OC)=O)[CH2:10][N:9]2[CH3:21])=[CH:5][CH:4]=1.[ClH:24]>CC(C)=O>[ClH:24].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][CH:8]2[C:13]([CH3:15])([CH3:14])[C:12](=[O:16])[CH2:11][CH2:10][N:9]2[CH3:21])=[CH:22][CH:23]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric Acid4회HCID 21448635Methyl 2-(p-methoxybenzyl)-4-oxo-1,3,3-trimethyl-5-piperidinecarboxylate

생성물 1

HCID 204746822-(p-Methoxybenzyl)-1,3,3-trimethyl-4-piperidone hydrochloride수율 87%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of the hydrochloride (80 g) of methyl 2-(p-methoxybenzyl)-4-oxo-1,3,3-trimethyl-5-piperidinecarboxylate in 450 ml of 1 N hydrochloric acid is refluxed for 12 hours. After cooling, some resinous material is removed by extraction with ether. Alkalinization of the aqueus solution with the aid of ammonia causes the separation of the piperidone which is extracted with ether. Concentration in vacuo of the extent gives a residue which is dissolved in ethanolic hydrogen chloride. Evaporation of the ethanol leaves a syrupy residue which is dissolved in acetone, whereafter the crystalline hydrochloride separates. Yield 87%. Melting point 168° - 170° C, with decomposition.

후처리

  1. temperatureAfter cooling
  2. customsome resinous material is removed by extraction with ether
  3. customthe separation of the piperidone which
  4. extractionis extracted with ether
  5. concentrationConcentration in vacuo of the extent
  6. customgives a residue which
  7. customEvaporation of the ethanol
  8. customleaves a syrupy residue which

출처 및 근거

ORD 기록
ord-9aabc34d04624859928ec041e070f79f
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012392

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