반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([C:17]2[CH:22]=[C:21]([C:23]([F:26])([F:25])[F:24])[CH:20]=[CH:19][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]=[C:21]([C:23]([F:26])([F:25])[F:24])[CH:20]=[CH:19][C:18]=3[O:16][N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]참가 물질
4
반응물 2
생성물 1
시약·촉매·용매 1
실험 절차
A solution of 4-[(2-Fluoro-5-trifluoromethyl-phenyl)-hydroxyimino-methyl]-piperidine-1-carboxylic acid tert-butyl ester (4.969 g, 0.013 M) in anhydrous THF (59 mL) was treated with Potassium tert-butoxide (13.4 mL of a 1M solution in THF, 0.0133 M-1.05 eq). The mixture was stirred at ambient temperature for 1 hour and then heated to 65° C. for 2 hours. The THF was removed under reduced pressure. The residue was dissolved in ethyl acetate (100 mL), washed with H2O (50 mL) and brine (50 mL) respectively. It was then dried over MgSO4, filtered and concentrated to give a solid (5 g) which was purified on silica ˜120 g, (eluting with ethylacetate heptane (30:70) to give the product as a white solid (2.69 g, 57%).
후처리
- temperatureheated to 65° C. for 2 hours
- customThe THF was removed under reduced pressure
- dissolutionThe residue was dissolved in ethyl acetate (100 mL)
- washwashed with H2O (50 mL) and brine (50 mL) respectively
- dry with materialIt was then dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-cc987dde104b489ab6857cf32d915e8a
- 출처 데이터셋
- uspto-grants-2010_08
- 특허 번호
- US07772252B2
연결된 노트
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