Acetic Acid → 5-methyl-5,6,7,8-tetrahydro-1,6-naphthyridine
反応式
[N+:1]([CH3:4])([O-])=O.[NH:5]1[CH2:10][CH2:9]CCC1.C(O)(=O)C.[CH:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>>[CH3:9][CH:10]1[NH:5][CH2:16][CH2:17][C:18]2[N:1]=[CH:4][CH:15]=[CH:20][C:19]1=2参加物
5
実験手順
To a solution of aldehyde A (1 mol) in benzene (approx. 20 ml per 1 g of the starting compound) nitromethane (1.2 mol), piperidine (0.1 mol) and acetic acid (0.1 mol) are added. The reaction mixture is refluxed for 2.5 h with azeotrope removing of water. Then, the solvent is evaporated in vacuo. The residue is triturated with cold methanol, filtered, washed with cold methanol that resulted in product crystals in good to moderate yields.
後処理
- temperatureThe reaction mixture is refluxed for 2.5 h with azeotrope
- customremoving of water
- customThen, the solvent is evaporated in vacuo
- customThe residue is triturated with cold methanol
- filtrationfiltered
- washwashed with cold methanol that
- customresulted in product crystals in good to moderate yields
出典と根拠
- ORDレコード
- ord-f8d440ea64f7407faab9167f63e427fb
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07985753B2
反応ノート
読み込み中…