4-Nitro-1-p-tolyl-1H-pyrazole → 4-Amino-1-p-tolyl-1H-pyrazole
반응식
[N+:1]([C:4]1[CH:5]=[N:6][N:7]([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=2)[CH:8]=1)([O-])=O>C(O)C.[Pd]>[NH2:1][C:4]1[CH:5]=[N:6][N:7]([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=2)[CH:8]=1참가 물질
4
실험 절차
Intermediate 6a (212 mg, 1.04 mmol) was dissolved in ethanol (20 mL) then hydrogenated over 10% palladium on carbon for 4 h under hydrogen atmosphere. The mixture was then filtered through Celite, washing with ethanol, and evaporated to dryness. The residue was purified by FCC, eluting with 0-10% MeOH in DCM, to give the title compound as a pale brown solid (154 mg, 86%). LCMS (Method 3): Rt 1.92 min, m/z 174.1 [MH−].
후처리
- filtrationThe mixture was then filtered through Celite
- washwashing with ethanol
- customevaporated to dryness
- customThe residue was purified by FCC
- washeluting with 0-10% MeOH in DCM
출처 및 근거
- ORD 기록
- ord-0c801d1a29f146f18c30dbeba6254041
- 출처 데이터셋
- uspto-grants-2015_05
- 특허 번호
- US09029373B2
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