2-Methyl-2-(4-nitro-pyrazol-1-yl)-propan-1-ol → 2-(4-amino-1H-pyrazol-1-yl)-2-methylpropan-1-ol
반응식
[CH3:1][C:2]([N:6]1[CH:10]=[C:9]([N+:11]([O-])=O)[CH:8]=[N:7]1)([CH3:5])[CH2:3][OH:4]>C(O)C.[C].[Pd]>[NH2:11][C:9]1[CH:8]=[N:7][N:6]([C:2]([CH3:5])([CH3:1])[CH2:3][OH:4])[CH:10]=1참가 물질
4
실험 절차
To a solution of the crude 2-methyl-2-(4-nitro-1H-pyrazol-1-yl)propan-1-ol (36 g) obtained in Step G of Example 103 in ethanol (200 mL) was added 10% palladium-carbon (360 mg), and the mixture was stirred overnight at room temperature under hydrogen atmosphere (at normal pressure). The palladium-carbon was removed by filtration through Celite, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/methanol), and the obtained solid was washed with diisopropyl ether to give the title compound (15 g).
후처리
- customThe palladium-carbon was removed by filtration through Celite
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (ethyl acetate/methanol)
- washthe obtained solid was washed with diisopropyl ether
출처 및 근거
- ORD 기록
- ord-f0cd1734c66e499e8cf662ebed5eaa12
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09187453B2
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