HCID 178482203、化合物 → HCID 178482196、化合物
反応式
[CH3:1][NH:2][C:3]1[CH:20]=[CH:19][C:18]([N+:21]([O-])=O)=[CH:17][C:4]=1[C:5]([N:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([OH:16])=[N:8]1)=[O:6]>CCO.[Pd]>[CH3:1][NH:2][C:3]1[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][C:4]=1[C:5]([N:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([OH:16])=[N:8]1)=[O:6]参加物
4
実験手順
To 1.1 g. of 1-(2-methylamino-5-nitrobenzoyl)-1H-indazol-3-ol, prepared in Example 14, suspended in 200 ml of absolute EtOH was added 200 mg of 5% Pd/C and the mixture was hydrogenated at 50 psi for 16 hours. The catalyst was filtered off, washed with hot EtOH and the filtrate was diluted with H2O and concentrated to small volume. The precipitate was collected, washed with cold 95% EtOH and dried; yield of dark-yellow amorphous powder 0.65 g. (65.4%); m.p. 184°-186° C.
後処理
- filtrationThe catalyst was filtered off
- washwashed with hot EtOH
- additionthe filtrate was diluted with H2O
- concentrationconcentrated to small volume
- customThe precipitate was collected
- washwashed with cold 95% EtOH
- customdried
出典と根拠
- ORDレコード
- ord-2e1ea073a0d54675ae6a193630976836
- 出典データセット
- uspto-grants-1985_08
- 特許番号
- US04537966
反応ノート
読み込み中…