Ethyl Acetate → 1-(1-Benzylpiperidin-4-yl)ethanone

HRID 887378ノート

反応式

HRID 887378 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](N(OC)C)=[O:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:20][Mg]Br.CCOC(C)=O.[NH4+].[Cl-]>C(OCC)C>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=[O:15])[CH3:20])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 25517Ammonium ChlorideHCID 211930301-benzyl-N-methoxy-N-methylpiperidine-4-carboxamideHCID 178418573HCID 178418573、化合物

生成物 1

HCID 9109231-(1-Benzylpiperidin-4-yl)ethanone

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
27.5 °C

実験手順

To a stirred solution of 1-benzyl-N-methoxy-N-methylpiperidine-4-carboxamide (11.5 g, 44 mmol) in diethyl ether (150 mL) at 0° C. was added methyl magnesium bromide (15.7 g, 132 mmol), drop-wise over 10 min. The resulting mixture was stirred at 25-30° C. for 2 h. After completion of the reaction, the mixture was treated with EtOAc and saturated NH4Cl solution. The separated organic layer was washed with brine and dried over anhydrous sodium sulfate and concentrated under vacuum to afford 1-(1-benzylpiperidin-4-yl)ethanone product. [M+1]=218.1

後処理

  1. customAfter completion of the reaction
  2. washThe separated organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-f2d4fe5c3c7f4c04977529d2f4e1cfcc
出典データセット
uspto-grants-2012_08
特許番号
US08247418B2

反応ノート

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