Water → 4-Hydroxymethyl-2-methoxy-3,5,6-trifluoropyridine
反応式
[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]参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-196ca99cd6fc42e5bb3bc6aab511676f
- 出典データセット
- uspto-grants-1987_10
- 特許番号
- US04701464
反応ノート
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