3-(Methylamino)-1-benzoxepin-5(2H)-one → HCID 13446113、化合物
反応式
[CH3:1][NH:2][C:3]1[CH2:4][O:5][C:6]2[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=2[C:8](=[O:10])[CH:9]=1.[H][H]>[Ni].C(O)C>[CH3:1][NH:2][CH:3]1[CH2:9][CH:8]([OH:10])[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[O:5][CH2:4]1参加物
5
実験手順
18.8 g (0.1 mole) 3-methylamino-1-benzoxepin-5(2H)-one is stirred with 40 g Raney Nickel in 400 ml ethanol for five hours at an hydrogen pressure of 55 bar. Subsequently, the catalyst is filtered out, the solvent is distilled off and one obtains 7.7 g (40% of the theoretical yield) racemic-2,3,4,5-tetrahydro-3-methylamino-1-benzoxepin-5-ol as an oil. The compound can be further separated as described earlier and further identified.
後処理
- filtrationSubsequently, the catalyst is filtered out
- distillationthe solvent is distilled off
- customone obtains 7.7 g (40% of the
出典と根拠
- ORDレコード
- ord-b943c0d410744239aaebae8c2953c235
- 出典データセット
- uspto-grants-1981_07
- 特許番号
- US04279904
反応ノート
読み込み中…