반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[C:18]=2F)=[N:15][OH:16])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CC(C)([O-])C.[K+]>C1COCC1>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[C:18]=3[O:16][N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]참가 물질
반응물 2
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 60 °C
실험 절차
To a room temperature mixture of 4-[(2-fluoro-3-trifluoromethyl-phenyl)-hydroxyimino-methyl]-piperidine-1-carboxylic acid tert-butyl ester (1.40 g, 3.59 mmol) in THF (20 mL) under nitrogen was added potassium tert-butoxide (3.60 mL of a 1 M THF solution, 3.60 mmol) in one portion and the reaction heated at 60° C. for 1.5 h. After standing at room temperature overnight, the solvent was removed and the residue diluted with ethyl acetate (60 mL). The organics were washed with water (30 mL) and brine (30 mL) successively, dried over magnesium sulfate, filtered, and concentrated to give an amber solid. The crude product was chromatographed on silica using 40% ethyl acetateiheptane as eluent to afford 0.97 g (73%) of the desired product as a white solid, mp:111–113° C.
후처리
- customthe solvent was removed
- additionthe residue diluted with ethyl acetate (60 mL)
- washThe organics were washed with water (30 mL) and brine (30 mL) successively
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customto give an amber solid
- customThe crude product was chromatographed on silica using 40% ethyl acetateiheptane as eluent
출처 및 근거
- ORD 기록
- ord-ffa0b744d9e3421c86c0c64eb40f7672
- 출처 데이터셋
- uspto-grants-2007_03
- 특허 번호
- US07186724B2
연결된 노트
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