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

HRID 596867ノート

反応式

HRID 596867 の反応式
[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

参加物

4

反応物 2

HCID 313Hydrochloric Acid4 回HCID 21448635Methyl 2-(p-methoxybenzyl)-4-oxo-1,3,3-trimethyl-5-piperidinecarboxylate

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9aabc34d04624859928ec041e070f79f
出典データセット
uspto-grants-1977_03
特許番号
US04012392

反応ノート

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