Hydrogen Peroxide → HCID 59634007、化合物
反応式
[Si:1]([O:8][CH2:9][C:10]([C:13]1[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=1)([F:12])[F:11])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[OH:19]O.O>C(Cl)(Cl)Cl.C[Re](=O)(=O)=O.[O-2].[Mn+4].[O-2]>[Si:1]([O:8][CH2:9][C:10]([C:13]1[CH:18]=[CH:17][N+:16]([O-:19])=[CH:15][CH:14]=1)([F:12])[F:11])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]参加物
7
実験手順
To a solution of 4-[2-(tert-butyldimethylsilanyloxy)-1,1-difluoroethyl]pyridine (0.14 g) prepared in (3) in chloroform (3 mL) were added methyltrioxorhenium (VII) (0.0010 g) and aqueous 30% hydrogen peroxide (0.11 mL). The reaction mixture was stirred at RT for 4 hr. To the mixture was added manganese (IV) oxide. The reaction mixture was stirred at RT for 1 hr. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was dried over MgSO4. The solvent was removed under reduced pressure to give the crude title compound.
後処理
- stirringThe reaction mixture was stirred at RT for 1 hr
- extractionthe mixture was extracted with ethyl acetate
- dry with materialThe organic layer was dried over MgSO4
- customThe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-2bb54548753147d6be282a2d499fa580
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08765739B2
反応ノート
読み込み中…