HCID 131735472、化合物 → HCID 76847321、化合物
反応式
[Cl:1][C:2]1[C:3]([CH:13]=[CH:14][N:15](C)C)=[C:4]([N+]([O-])=O)[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[H][H]>C(OCC)(=O)C.[Ni]>[Cl:1][C:2]1[CH:7]=[N:6][C:5]([O:8][CH3:9])=[C:4]2[NH:15][CH:14]=[CH:13][C:3]=12参加物
5
実験手順
To a solution of Example 108C (12 g, 46.6 mmol) in ethyl acetate (150 mL) was added Raney-Ni (20.0 g, 4.66 mmol), and the reaction mixture was stirred for 20 hours at room temperature under 30 atm. hydrogen. The reaction mixture was filtered and rinsed with ethyl acetate. The filtrate was concentrated to a small volume, and the precipitates were collected by filtration and dried to provide the title compound (10 g, 93% yield).
後処理
- filtrationThe reaction mixture was filtered
- washrinsed with ethyl acetate
- concentrationThe filtrate was concentrated to a small volume
- filtrationthe precipitates were collected by filtration
- customdried
出典と根拠
- ORDレコード
- ord-dcae7173ec4c4e5c95afe1a6aa561342
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09321764B2
反応ノート
読み込み中…