Methanol → Methyl 2-chloro-5-methoxy-4-nitrobenzoate
反応式
[Cl:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([O:14][CH3:15])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH3:21]O>>[Cl:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([O:14][CH3:15])=[CH:7][C:3]=1[C:4]([O:6][CH3:21])=[O:5]参加物
4
実験手順
A solution of 2-chloro-5-methoxy-4-nitrobenzoic acid (1 mmol) and concentrated sulfuric acid (0.02 mmol) in methanol (200 mL) was heated to reflux for 42 hours. The solvents were evaporated under reduced pressure then the residue partitioned between EtOAc (25 mL) and water (25 mL). The separated aqueous phase was extracted with EtOAc (3×25 mL), then the combined organic extracts were dried (Na2SO4) and concentrated under reduced pressure to afford the title compound (71%) as a solid.
後処理
- temperatureto reflux for 42 hours
- customThe solvents were evaporated under reduced pressure
- customthe residue partitioned between EtOAc (25 mL) and water (25 mL)
- extractionThe separated aqueous phase was extracted with EtOAc (3×25 mL)
- dry with materialthe combined organic extracts were dried (Na2SO4)
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-e3c0aea2e8f442948cbd6ab9ff921168
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08716287B2
反応ノート
読み込み中…