Hydrochloric Acid → Benzoic acid, 4-amino-3-nitro-, ethyl ester
反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].Cl.[CH2:15](O)[CH3:16]>CCOCC>[CH2:15]([O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([NH2:1])=[C:3]([N+:11]([O-:13])=[O:12])[CH:4]=1)[CH3:16]参加物
5
実験手順
4-Amino-3-nitrobenzoic acid (5.0 g, 27.4 mmol) was dissolved in ethanol (100 mL) and treated with a 2N solution of HCl in ether (30 mL). The reaction mixture was refluxed for 16 h, then the solvent was removed in vacuo. The crude compound was dissolved in dichloromethane and washed with NaOH 0.5N. The organic phase was dried over sodium sulfate and the solvent was removed. 4-Amino-3-nitrobenzoic acid ethyl ester was thus obtained as a yellow solid, 4.6 g, (79%), MS (ISP): m/e=211.1 (M+H+.), and used crude in the following reaction.
後処理
- temperatureThe reaction mixture was refluxed for 16 h
- customthe solvent was removed in vacuo
- dissolutionThe crude compound was dissolved in dichloromethane
- washwashed with NaOH 0.5N
- dry with materialThe organic phase was dried over sodium sulfate
- customthe solvent was removed
出典と根拠
- ORDレコード
- ord-b83e5d9ca64245829231f6e65aacbacf
- 出典データセット
- uspto-grants-2011_10
- 特許番号
- US08030308B2
反応ノート
読み込み中…