Stannous chloride dihydrate → 1-(3,4-diaminophenyl)ethanone
反応式
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[C:6]([N+:11]([O-])=O)[CH:5]=1)=[O:3].O.O.Cl[Sn]Cl.C([O-])(O)=O.[Na+]>CCOC(C)=O.O>[NH2:11][C:6]1[CH:5]=[C:4]([C:2](=[O:3])[CH3:1])[CH:9]=[CH:8][C:7]=1[NH2:10]参加物
6
実験手順
To a solution of 4-methylcarbonyl-2-nitro-benzenamine (500 mg, 2.775 mmol) in EtOAc (16 mL) was added SnCl2.2H2O (3.130 g, 13.88 mmol). The reaction mixture was refluxed for 2.5 h, cooled to rt, and diluted with H2O (130 mL). The pH of the mixture was adjusted to 7-8 by addition of saturated NaHCO3 solution and the aqueous phase was extracted with EtOAc (2×120 mL). The combined organic extracts were washed with brine (2×60 mL) and dried over MgSO4. After the removal of the solvent under vacuum, 142a was obtained as a red orange solid (418 mg).
後処理
- temperatureThe reaction mixture was refluxed for 2.5 h
- extractionthe aqueous phase was extracted with EtOAc (2×120 mL)
- washThe combined organic extracts were washed with brine (2×60 mL)
- dry with materialdried over MgSO4
- customAfter the removal of the solvent under vacuum
出典と根拠
- ORDレコード
- ord-ca0b7a9dd9b24df397a66ed41808e721
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08053450B2
反応ノート
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