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

HRID 2191918노트

반응식

HRID 2191918 반응식
[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

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 25517Ammonium ChlorideHCID 211930301-benzyl-N-methoxy-N-methylpiperidine-4-carboxamideHCID 178418573HCID 178418573, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
27.5 °C

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-ec427f758b47444bafc049ea09cbb313
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329700B2

반응 노트

불러오는 중…