Hydrogen Peroxide → 4-[2-(4-Fluoro-phenyl)-1,1-dimethoxy-ethyl]-pyridine 1-oxide

HRID 659949

反応式

HRID 659949 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)([O:12][CH3:13])[O:10][CH3:11])=[CH:4][CH:3]=1.[OH:20]O>ClCCl.C[Re](=O)(=O)=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([C:14]2[CH:15]=[CH:16][N+:17]([O-:20])=[CH:18][CH:19]=2)([O:10][CH3:11])[O:12][CH3:13])=[CH:4][CH:3]=1

参加物

5

実験手順

55 g (0.21 mole) of 4-[2-(4-Fluoro-phenyl)-1,1-dimethoxy-ethyl]-pyridine and 445 mg of methyltrioxorhenium are dissolved in 250 mL of dichloromethane. 112 mL of commercial hydrogen peroxide solution is added to the reaction mixture which is further stirred over night at room temperature. The reaction mixture is then decanted and the organic phase is washed with sodium hydrogen sulfate and water and dried over magnesium sulfate. After concentration, 33 g of 4-[2-(4-Fluoro-phenyl)-1,1-dimethoxy-ethyl]-pyridine 1-oxide is obtained as a green oil.

後処理

  1. customThe reaction mixture is then decanted
  2. washthe organic phase is washed with sodium hydrogen sulfate and water
  3. dry with materialdried over magnesium sulfate
  4. concentrationAfter concentration

出典と根拠

ORDレコード
ord-fae9c6c33f6a453e8bf832c89648a41c
出典データセット
uspto-grants-2011_12
特許番号
US08084395B2

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