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Sodium Bicarbonate → 6-Methoxy-3,3-dimethyl-2,3,4,5-tetrahydropyridine

HRID 1158906
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HRID 1158906 반응식
F[B-](F)(F)F.[CH3:6][O+:7]([CH3:9])C.[CH3:10][C:11]1([CH3:18])[CH2:16][NH:15]C(=O)[CH2:13][CH2:12]1.C(=O)([O-])O.[Na+]>ClCCl>[CH3:10][C:11]1([CH3:18])[CH2:12][CH2:13][C:6]([O:7][CH3:9])=[N:15][CH2:16]1
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참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 104796605,5-Dimethylpiperidin-2-one

생성물 1

HCID 219413936-Methoxy-3,3-dimethyl-2,3,4,5-tetrahydropyridine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trimethyloxonium tetrafluoroborate (97%, 11.9 g, 78 mmol) was added to the dry dichloromethane (156 mL) solution of 5,5-dimethyl-2-piperidone (9.93 g, 78 mmol) at room temperature and stirred for 14 h. The reaction mixture was neutralized with 10% sodium hydrogen carbonate aqueous solution, and the organic layer was separated. The aqueous layer was extracted with ethyl acetate (3×120 mL), then the combined organic layer was washed with 10% sodium hydrogen carbonate aqueous solution and brine. The organic layer was dried (MgSO4) and filtered. The filtrate was concentrated under reduced pressure and the titled compound was obtained as pale yellow oil (9.0 g, 82.0%).

후처리

  1. customthe organic layer was separated
  2. extractionThe aqueous layer was extracted with ethyl acetate (3×120 mL)
  3. washthe combined organic layer was washed with 10% sodium hydrogen carbonate aqueous solution and brine
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1dfd0b673eb8446dba5dfdb77a71bfea
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07812014B2

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