반응식
[F:1][C:2]([F:31])([F:30])[C:3](O)(O)[CH:4]([O:11][C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[N:17]([C:21]1[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=1)[N:16]=[CH:15]2)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl.[NH2:33][OH:34]>N1C=CC=CC=1>[F:1][C:2]([F:31])([F:30])[C:3](=[N:33][OH:34])[CH:4]([O:11][C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[N:17]([C:21]1[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=1)[N:16]=[CH:15]2)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1참가 물질
반응 조건
- 온도
- 115 °C
실험 절차
1,1,1-trifluoro-3-(1-(4-fluorophenyl)-1H-indazol-5-yloxy)-3-phenylpropane-2,2-diol (147c) 1.22 g, 2.8 mmol) and hydroxylamine hydrochloride (3.32 g, 48 mmol) was mixed in pyridine (85 mL, dried over 4 Å MS). The mixture was stirred at 115° C. for 30 min, after which time HPLC analysis showed complete reaction. Solvent was evaporated and the residue partitioned between ethyl acetate and water. The phases were separated and the organic phase washed twice with water, followed by brine and then evaporated. The residue was subjected to chromatography (SiO2, gradient of 10-60% Ethyl acetate in Heptane) to afford somewhat impure 1,1,1-trifluoro-3-(1-(4-fluorophenyl)-1H-indazol-5-yloxy)-3-phenylpropan-2-one oxime as a 3:7 mixture of diastereomers (0.99 g, 82%).
후처리
- customreaction
- customSolvent was evaporated
- customthe residue partitioned between ethyl acetate and water
- customThe phases were separated
- washthe organic phase washed twice with water
- customevaporated
출처 및 근거
- ORD 기록
- ord-c646ec47c78349c494c33ff3e9e59ec1
- 출처 데이터셋
- uspto-grants-2012_03
- 특허 번호
- US08143290B2
연결된 노트
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