1-Benzyl-4-piperidone → 1-Benzyl-4-methylpiperidin-4-ol

HRID 238286ノート

反応式

HRID 238286 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:15][Mg]Br.[Cl-].[NH4+]>C1COCC1.CCOCC>[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]([CH3:15])([OH:14])[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 192201-Benzyl-4-piperidoneHCID 25517Ammonium ChlorideHCID 178418573HCID 178418573、化合物

生成物 1

HCID 108459131-Benzyl-4-methylpiperidin-4-ol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1-benzyl-4-piperidone (26.5 mmol, 5 g) in THF (50 mL) was cooled to −15° C. and a solution of methyl magnesium bromide in ether (3 M, 22 mL) was added. The mixture was stirred for 0.5 hours then allowed to warm to room temperature. Saturated aqueous ammonium chloride (50 mL) was added and the products were extracted into ethyl acetate, dried over magnesium sulphate, filtered and the solvent removed by evaporation under vacuum to give the title compound as a pale yellow solid (5.0 g) that was used directly without further purification.

後処理

  1. extractionthe products were extracted into ethyl acetate
  2. dry with materialdried over magnesium sulphate
  3. filtrationfiltered
  4. customthe solvent removed by evaporation under vacuum

出典と根拠

ORDレコード
ord-7c4bdb5ed68c4c7db9fbbf0069da3577
出典データセット
uspto-grants-2014_02
特許番号
US08642621B2

反応ノート

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