Hydrazine hydrate (1:1) → HCID 57423910、化合物
反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N+:22]([O-])=O)=[C:6]([NH:8][CH:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)[CH:7]=1.O.NN>C(O)C.[Ni]>[NH2:22][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][C:6]=1[NH:8][CH:9]1[CH2:10][CH2:11][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:13][CH2:14]1参加物
5
反応条件
- 温度
- 40 °C
実験手順
1,1-Dimethylethyl 4-[(5-chloro-2-nitrophenyl)amino]-piperidinecarboxylate D27 (6.3 g) was dissolved in ethanol (100 mL) and Raney nickel (50% aqueous suspension, 5 mL) was added at room temperature; the mixture was heated to 40° C. and hydrazine monohydrate (3.0 mL) was added over 30 min. After 30 min more, the reaction mixture was cooled to room temperature, filtered through Celite and the solvent was evaporated to yield the title compound, 5.8 g.
後処理
- temperaturethe reaction mixture was cooled to room temperature
- filtrationfiltered through Celite
- customthe solvent was evaporated
出典と根拠
- ORDレコード
- ord-41d00deec6a54e2bbdeab187f2b94f72
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08288413B2
反応ノート
読み込み中…