Methanol → Methyl 3-bromo-2-methoxybenzoate
反応式
S(=O)(=O)(O)O.[Br:6][C:7]1[C:8]([O:16][CH3:17])=[C:9]([CH:13]=[CH:14][CH:15]=1)[C:10]([OH:12])=[O:11].[CH3:18]O>>[CH3:18][O:11][C:10](=[O:12])[C:9]1[CH:13]=[CH:14][CH:15]=[C:7]([Br:6])[C:8]=1[O:16][CH3:17]参加物
4
実験手順
5.0 mL of sulfuric acid (H2SO4) was slowly added to a solution of 5.0 g of 3-bromo-2-methoxy-benzoic acid 4 in 100 mL of methanol (MeOH). The resulting solution was heated to reflux overnight. The solution was cooled to room temperature and quenched with sodium bicarbonate to pH 7. The aqueous layer was extracted several times with ethyl acetate. The combined organic extracts were washed with brine and dried over sodium sulphate. The resulting mixture was filtered. The solvents were evaporated under reduced pressure to afford 5.3 g of 3-bromo-2-methoxy-benzoic acid methyl ester 5.
後処理
- temperatureThe resulting solution was heated
- temperatureto reflux overnight
- customquenched with sodium bicarbonate to pH 7
- extractionThe aqueous layer was extracted several times with ethyl acetate
- washThe combined organic extracts were washed with brine
- dry with materialdried over sodium sulphate
- filtrationThe resulting mixture was filtered
- customThe solvents were evaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-9241bc404e4f49a2bc303f319c431a23
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08071636B2
反応ノート
読み込み中…