5-chloro-4-nitro-1H-indazole → 5-Chloro-1H-indazol-4-amine
反応式
[Cl:1][C:2]1[C:3]([N+:11]([O-])=O)=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][N:6]=[CH:5]2>[Pd]>[Cl:1][C:2]1[C:3]([NH2:11])=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][N:6]=[CH:5]2参加物
3
実験手順
A solution that consists of 5-chloro-4-nitro-1H-indazole (872 mg, 4.41 mmol) is mixed with 150 mg of palladium on carbon (10%) and stirred under hydrogen atmosphere at room temperature. After 45 minutes, the catalyst is suctioned off on one frit and washed with methanol. The filtrate is concentrated by evaporation, and the residue is taken up in 200 ml of ethyl acetate and heated. After renewed suctioning-off and concentration by evaporation of the filtrate, the purification on silica gel is carried out with hexane/ethyl acetate (100-33% hexane). 296 mg (40% of theory) of the product is obtained.
後処理
- washwashed with methanol
- concentrationThe filtrate is concentrated by evaporation
- temperatureheated
- concentrationconcentration
- customby evaporation of the filtrate
- customthe purification on silica gel
- custom296 mg (40% of theory) of the product is obtained
出典と根拠
- ORDレコード
- ord-4c2200109c0749ffab074f3e8178619f
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07662821B2
反応ノート
読み込み中…