Acetone → Methyl 3-fluoro-2-methoxybenzoate
反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:4]([C:5](O)=[O:6])[C:3]=1O.IC.[C:14](=[O:17])([O-])[O-].[K+].[K+].[CH3:20]C(C)=O.[OH2:24]>>[F:1][C:2]1[C:3]([O:17][CH3:14])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([O:6][CH3:20])=[O:24]参加物
6
実験手順
A mixture containing 3-fluorosalicylic acid (20 g) [obtained as white crystals, m.p. 145°-147° C., by the method of L N Ferguson et alia, J.Amer.Chem.Soc., 1950, 72, 5315], iodomethane (60 g), potassium carbonate (40 g) and acetone (200 ml) was heated under reflux for 24 hours. Water (500 ml) was added and the mixture was extracted with ether (3×150 ml). The combined extracts were dried (MgSO4) and evaporated to give methyl 3-fluoro-2-methoxybenzoate (B) (21 g) as a yellow oil, which was used without further purification; NMR: 3.85 (3H,s), 3.95 (3H,s) and 6.8-7.6 (3H,m).
後処理
- customobtained as white crystals, m.p. 145°-147° C., by the method of L N Ferguson et alia, J.Amer.Chem.Soc
- temperatureunder reflux for 24 hours
- extractionthe mixture was extracted with ether (3×150 ml)
- dry with materialThe combined extracts were dried (MgSO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-ba6defad96e244e392b8e5a6b7ec0a68
- 出典データセット
- uspto-grants-1990_03
- 特許番号
- US04908380
反応ノート
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