8-nitro-3,4-dihydro-2H-1,5-benzodioxepin-7-amine → 3,4-dihydro-2H-1,5-benzodioxepine-7,8-diamine
反応式
[NH2:1][C:2]1[C:12]([N+:13]([O-])=O)=[CH:11][C:5]2[O:6][CH2:7][CH2:8][CH2:9][O:10][C:4]=2[CH:3]=1>CO.[Ni]>[O:6]1[C:5]2[CH:11]=[C:12]([NH2:13])[C:2]([NH2:1])=[CH:3][C:4]=2[O:10][CH2:9][CH2:8][CH2:7]1参加物
4
実験手順
10.2 g of 7-amino-8-nitro-3,4-dihydro-2H-1,5-benzodioxepine were hydrogenated in 500 ml of methanol with Raney-nickel. After separating the catalyst, the solution was evaporated and the residue was recrystallized from ethyl acetate/petroleum either (low boiling). 7.7 g of 3,4-dihydro-2H-1,5-benzodioxepine-7,8-diamine (88.0% of theory) of melting point 97°-102° C. were obtained.
後処理
- customAfter separating the catalyst
- customthe solution was evaporated
- customthe residue was recrystallized from ethyl acetate/petroleum either (low boiling)
出典と根拠
- ORDレコード
- ord-3177585f85e241dd95d124777ec85bd9
- 出典データセット
- uspto-grants-1985_11
- 特許番号
- US04554280
反応ノート
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