5-chloro-4-nitro-1H-indazole → 5-Chloro-1H-indazol-4-amine
반응식
[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]2참가 물질
3
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-8ec87901cb0c4796b9a0c1d7c65f51b7
- 출처 데이터셋
- uspto-grants-2009_12
- 특허 번호
- US07638515B2
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