Methanol → Methyl 4-nitroanthranilate
反応式
[NH2:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:19]O>>[NH2:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:19])=[O:5]参加物
4
実験手順
A mixture of 118.8 g of 2-amino-4-nitro-benzoic acid, 1000 ml of methanol and 120 ml of concentrated sulfuric acid is heated at the boiling point for 16 hours. The mixture is concentrated under reduced pressure, the residue is taken up in ethyl acetate and the mixture is washed with saturated NaHCO3 solution. After drying over Na2SO4, the organic phase is concentrated. 114.2 g (89%) of methyl 2-amino-4-nitro-benzoate are thus obtained with a melting point (m.p.) of 156-158° C.
後処理
- temperatureis heated at the boiling point for 16 hours
- concentrationThe mixture is concentrated under reduced pressure
- washthe mixture is washed with saturated NaHCO3 solution
- dry with materialAfter drying over Na2SO4
- concentrationthe organic phase is concentrated
出典と根拠
- ORDレコード
- ord-4f8c35cb17de4c0ca3cb4158075d7987
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05922646
反応ノート
読み込み中…