Water → 4-Hydroxymethyl-2-methoxy-3,5,6-trifluoropyridine
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[OH:1][CH2:2][C:3]1[C:8]([F:9])=[C:7]([F:10])[N:6]=[C:5](F)[C:4]=1[F:12].[CH3:13][O-:14].[Na+].O>CO>[OH:1][CH2:2][C:3]1[C:8]([F:9])=[C:7]([F:10])[N:6]=[C:5]([O:14][CH3:13])[C:4]=1[F:12]참가 물질
5
실험 절차
A mixture of 1.0 g (0.0055 mole) of 4-hydroxymethyl-2,3,5,6-tetrafluoropyridine (from Example 5) and 0.30 g (0.0055 mole) of sodium methoxide in 25 ml of methanol was refluxed for approximately twenty hours. After being cooled, the reaction mixture was poured into water. The aqueous solution was extracted with diethyl ether. The diethyl ether extract was dried over anhydrous magnesium sulfate, filtered, and the solvent evaporated under reduced pressure, yielding 0.85 g of 4-hydroxymethyl-2-methoxy-3,5,6-trifluoropyridine as a yellow oil. The structure and nmr spectra are set forth in Table 1C below.
후처리
- temperaturewas refluxed for approximately twenty hours
- temperatureAfter being cooled
- extractionThe aqueous solution was extracted with diethyl ether
- extractionThe diethyl ether extract
- dry with materialwas dried over anhydrous magnesium sulfate
- filtrationfiltered
- customthe solvent evaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-196ca99cd6fc42e5bb3bc6aab511676f
- 출처 데이터셋
- uspto-grants-1987_10
- 특허 번호
- US04701464
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