Methanol → Methyl 5-fluoro-2-iodobenzoate
反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([I:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].OS(O)(=O)=O.[OH-].[Na+].[CH3:19]O>>[CH3:19][O:8][C:7](=[O:9])[C:6]1[CH:10]=[C:2]([F:1])[CH:3]=[CH:4][C:5]=1[I:11]参加物
5
実験手順
A mixture of 5-fluoro-2-iodo-benzoic acid (10.05 g, 39.47 mmol) and conc. H2SO4 (10 mL) in MeOH (100 ml) was reflux for 6 hours. After cooling to room temperature, NaOH (2N) was added dropwise to adjust the pH˜8. After most of organic solvent was removed under reduced pressure, the mixture was extracted with dichloromethane three times. The combined organic layers were washed with water, dried and concentrated to give the titled compound (10.80 g, yield 98%)
後処理
- temperaturewas reflux for 6 hours
- customAfter most of organic solvent was removed under reduced pressure
- extractionthe mixture was extracted with dichloromethane three times
- washThe combined organic layers were washed with water
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-b809cd07a3684f20b019cadc15329a29
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08431581B2
反応ノート
読み込み中…