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

HRID 1158906
ノート
印刷プレビュー

反応式

HRID 1158906 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-1dfd0b673eb8446dba5dfdb77a71bfea
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07812014B2

反応ノート

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