p-Toluenesulfonic acid monohydrate → HCID 59216307、化合物
反応式
[F:1][C:2]1[CH:11]=[C:10]([C:12](=[O:15])[CH:13]=[O:14])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C([O-])([O-])[O:17][CH2:18][CH3:19].O.[C:23]1(C)C=CC(S(O)(=O)=O)=C[CH:24]=1>C1(C)C=CC=CC=1>[CH2:23]([O:14][CH:13]([O:17][CH2:18][CH3:19])[C:12]([C:10]1[CH:9]=[CH:8][C:3]([C:4]([O:6][CH3:7])=[O:5])=[C:2]([F:1])[CH:11]=1)=[O:15])[CH3:24]参加物
5
実験手順
A mixture of methyl 2-fluoro-4-(oxoacetyl)benzoate (1.60 g), ethyl orthoformate (5.2 mL), p-toluenesulfonic acid monohydrate (70 mg) in toluene (20 mL) was heated under reflux for 3 h. After cooling, the mixture was concentrated. The residue was flash chromatographed on a silica gel column to give the desired product (0.63 g).
後処理
- temperaturewas heated
- temperatureunder reflux for 3 h
- temperatureAfter cooling
- concentrationthe mixture was concentrated
- customchromatographed on a silica gel column
出典と根拠
- ORDレコード
- ord-23edba30ab2342fa86b6817af43d17f1
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08143251B2
反応ノート
読み込み中…