Tetrabutylammonium Fluoride → 2-(2,5-Difluoro-phenoxy)-ethanol
반응식
[F:1][C:2]1[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:3]=1[O:4][CH2:5][CH2:6][O:7][Si](C(C)C)(C(C)C)C(C)C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1>[F:1][C:2]1[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:3]=1[O:4][CH2:5][CH2:6][OH:7]참가 물질
4
반응 조건
- 온도
- 60 °C
실험 절차
The solution of 1.80 g of [2-(2,5-difluorophenoxy)ethoxy]triisopropylsilane and 23 ml of tetrahydrofuran is admixed with 4.37 ml of tetrabutylammonium fluoride solution (1M in tetrahydrofuran) and stirred at 60° C. over 1 hour. The reaction mixture is cooled, poured onto water (70 ml) and extracted with tert-butyl methyl ether (2×70 ml). The organic phases are washed with brine (1×50 ml), dried over sodium sulphate, filtered and concentrated by evaporation. The title compound is obtained as a colourless oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.19 (2:1 EtOAc-heptane); Rt=3.17.
후처리
- temperatureThe reaction mixture is cooled
- additionpoured onto water (70 ml)
- extractionextracted with tert-butyl methyl ether (2×70 ml)
- washThe organic phases are washed with brine (1×50 ml)
- dry with materialdried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated by evaporation
출처 및 근거
- ORD 기록
- ord-5a0a5d5d4e2e487bae23198f2a6713f0
- 출처 데이터셋
- uspto-grants-2010_11
- 특허 번호
- US07842688B2
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