Methanol → 3-Bromo-4-methoxyaniline
反応式
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][C:3]=1[O:11][CH3:12].O.O.Cl[Sn]Cl.CO.C([O-])(O)=O.[Na+]>CCOC(C)=O.O>[Br:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[O:11][CH3:12]参加物
7
実験手順
2-Bromo-1-methoxy-4-nitrobenzene (2.50 g, 10.8 mmol), SnCl2.2H2O (12.2 g, 53.9 mmol), and MeOH (30 mL) were combined and allowed to stir for 3 h at ambient temperature. To the mixture was added H2O (100 mL) and EtOAc (100 mL) resulting in the formation of a thick emulsion. To this was added sat. aq. NaHCO3 (30 mL). The layers were separated and the aqueous layer was extracted with EtOAc (3×30 mL). The organics were combined and dried over MgSO4 before being filtered. Concentration of the filtrate in vacuo gave 2.02 g of an off-white solid. This material was used without further purification.
後処理
- customresulting in the formation of a thick emulsion
- customThe layers were separated
- extractionthe aqueous layer was extracted with EtOAc (3×30 mL)
- dry with materialdried over MgSO4
- filtrationbefore being filtered
出典と根拠
- ORDレコード
- ord-a48eb89408e442eaa73e43e78766a091
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846753B2
反応ノート
読み込み中…