Methanol → Methyl 5-fluoro-2-iodobenzoate
反応式
[F:1][C:2]1[CH:3]=[C:4]([C:8]([I:11])=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:17]O>>[F:1][C:2]1[CH:3]=[C:4]([C:8]([I:11])=[CH:9][CH:10]=1)[C:5]([O:7][CH3:17])=[O:6]参加物
4
実験手順
To a solution of 3-fluoro-6-iodo benzoic acid (50 g; 0.18 mol) in methanol (220 ml) were added 10 ml of sulfuric acid and the mixture heated at reflux for 24 hours. After that the solvent was evaporated and the crude mixture diluted with water and extracted with dichloromethane (3×70 ml), the organic phases were collected, washed with bicarbonate (3×100 ml), dried over sodium sulphate and concentrated to yield the desired compound (51 g).
後処理
- temperaturethe mixture heated
- temperatureat reflux for 24 hours
- customAfter that the solvent was evaporated
- additionthe crude mixture diluted with water
- extractionextracted with dichloromethane (3×70 ml)
- customthe organic phases were collected
- washwashed with bicarbonate (3×100 ml)
- dry with materialdried over sodium sulphate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-bcac7cce355c41cc99d2ba55920fe80e
- 出典データセット
- uspto-grants-2015_06
- 特許番号
- US09062033B2
反応ノート
読み込み中…