Sodium Bicarbonate → 2'-Fluoro-2-(1-fluoro-3,3-dimethylbutyl)-5'-methoxy-4-((4-methoxybenzyl)oxy)biphenyl
반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21](OC)=[CH:20][CH:19]=2)=[CH:12][C:11]=1[CH:26](O)[CH2:27][C:28]([CH3:31])([CH3:30])[CH3:29].C(C1C=C(C)C(S(F)(F)[F:45])=C(C)C=1)(C)(C)C.[C:49](=[O:52])([O-])O.[Na+]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:52][CH3:49])=[CH:20][CH:19]=2)=[CH:12][C:11]=1[CH:26]([F:45])[CH2:27][C:28]([CH3:30])([CH3:31])[CH3:29]참가 물질
5
반응물 3
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 0 °C
실험 절차
To a solution of 1-(2′-fluoro-5′-methoxy-4-((4-methoxybenzyl)oxy)biphenyl-2-yl)-3,3-dimethylbutan-1-ol (220 mg) in toluene (5 mL) was added 4-(tert-butyl)-2,6-dimethylphenylsulfur trifluoride (188 mg) at 0° C., and the mixture was stirred at 0° C. for 20 min. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (180 mg) as a colorless oil.
후처리
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
출처 및 근거
- ORD 기록
- ord-e5e1f550820c4ab9a733d3a72a8b84f6
- 출처 데이터셋
- uspto-grants-2016_07
- 특허 번호
- US09382188B2
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