Acetonitrile → Bis(p-chlorophenyl)amine
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5](B(O)O)=[CH:4][CH:3]=1.NO.[ClH:13].C([O-])([O-])=O.[K+].[K+].[CH3:20][C:21]#[N:22]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:22][C:21]2[CH:4]=[CH:3][C:2]([Cl:13])=[CH:7][CH:20]=2)=[CH:4][CH:3]=1参加物
5
反応条件
- 温度
- 70 °C
実験手順
Under air, a 500-mL rbf was charged with (4-chlorophenyl)boronic acid (15.0 g, 96.0 mmol, 1 eq.), NH2OH.HCl (8.0 g, 115 mmol, 1.2 eq.), CuBr (2.75 g, 19.18 mmol, 0.2 eq.), K2CO3 (19.89 g, 144.0 mmol, 1.5 eq.), and CH3CN (320 mL). The reaction mixture was stirred at 70° C. for 24 h. The completion of the reaction was monitored by TLC. The solvent was evaporated under reduced pressure and the residue was purified by flash column chromatography on a silica gel using 10%-20% EtOAc in hexanes to give the product as brown oil that solidifies when dried under vacuum.
後処理
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by flash column chromatography on a silica gel using 10%-20% EtOAc in hexanes
出典と根拠
- ORDレコード
- ord-c8ffc496ff8a4f36a63686dc5a044e11
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09227986B2
反応ノート
読み込み中…