Dimethylformamide → Methyl 3-carbamoyl-5-nitrobenzoate
反応式
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([CH:11]=[C:12]([N+:14]([O-:16])=[O:15])[CH:13]=1)[C:8](O)=[O:9])=[O:4].O=S(Cl)Cl.C[N:22](C=O)C>>[CH3:1][O:2][C:3](=[O:4])[C:5]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[C:7]([C:8](=[O:9])[NH2:22])[CH:6]=1参加物
4
実験手順
A mixture of 3-methoxycarbonyl-5-nitrobenzoic acid (44 mmol), SOCl2 (40 mL) and DMF (1 mL) was heated to reflux for 2 hours. Then the excessive SOCl2 was removed under reduced pressure. The residue was dissolved in DCM (80 mL), and added with NH3.H2O (15 mL) dropwise after cooling by ice-water. After addition, it was continued to stir 5 min. The resulting mixture was filtrated to give methyl-3-carbamoyl-5-nitrobenzoate in 85% yield.
後処理
- temperaturewas heated
- temperatureto reflux for 2 hours
- customThen the excessive SOCl2 was removed under reduced pressure
- dissolutionThe residue was dissolved in DCM (80 mL)
- additionadded with NH3.H2O (15 mL) dropwise
- temperatureafter cooling by ice-water
- additionAfter addition, it
- filtrationThe resulting mixture was filtrated
出典と根拠
- ORDレコード
- ord-4ff90498172a4076bdb23340aa885828
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07868001B2
反応ノート
読み込み中…