Methanol → Methyl 1-cyclohexyl-6-oxo-1,6-dihydro-3-pyridinecarboxylate
反応式
O=[C:2]1[O:7][CH:6]=[C:5]([C:8]([O-:10])=[O:9])[CH:4]=[CH:3]1.[CH:11]1([NH2:17])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1.[CH3:18]O>>[CH:11]1([N:17]2[C:2](=[O:7])[CH:3]=[CH:4][C:5]([C:8]([O:10][CH3:18])=[O:9])=[CH:6]2)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1参加物
4
実験手順
To a solution of 6-oxo-6H-pyran-3-carboxylate (1.14 g, 7.4 mmol, Aldrich) and 20 mL of MeOH was added cyclohexylamine (2.50 mL, 21.9 mmol, Aldrich). The solution was stirred at reflux for 16 hours, then concentrated in vacuo. The crude material was chromatographed through a Redi-Sep® pre-packed silica gel column (12 g), eluting with 5% to 20% EtOAc:hexane to give 460 mg (26%) of the title compound as a dark yellow oil. MS m/z: 236.4 (M+1).
後処理
- temperatureat reflux for 16 hours
- concentrationconcentrated in vacuo
- customThe crude material was chromatographed through a Redi-Sep® pre-packed silica gel column (12 g)
- washeluting with 5% to 20% EtOAc
出典と根拠
- ORDレコード
- ord-ac954ef7d2cf4bdab733573a6f87e3e2
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08163766B2
反応ノート
読み込み中…