Methanol → Methyl 3-Amino-4-methoxybenzoate
反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:5]([OH:7])=[O:6].OS(O)(=O)=O.[CH3:18]O>>[CH3:18][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][C:10]([O:11][CH3:12])=[C:2]([NH2:1])[CH:3]=1参加物
4
実験手順
3-amino-4-methoxy benzoic acid (40 g, 0.239 mol) was dissolved in methanol, H2SO4 (38.14 ml, 0.717 mol) was added dropwise thereto and refluxed for 12 hours. The resulting mixture was cooled to room temperature and concentrated under a reduced pressure to remove methanol, neutralized with NaHCO3, extracted with ethyl acetate, and the extract was concentrated under a reduced pressure. The resulting residue was purified by recrystallization from ethyl acetate/hexane to obtain the title compound (39 g, 0.215 mol) in a yield of 90%.
後処理
- temperaturerefluxed for 12 hours
- concentrationconcentrated under a reduced pressure
- customto remove methanol
- extractionextracted with ethyl acetate
- concentrationthe extract was concentrated under a reduced pressure
- customThe resulting residue was purified by recrystallization from ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-56b670bf3a344ba1ad9a3b62c234d033
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07179832B2
反応ノート
読み込み中…