反応式
[F:1][CH:2]([F:26])[C:3]([CH3:25])([CH3:24])[CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([N:14]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)C(=O)C)[CH:8]=1.[OH-].[K+].C(O)C.C(OCC)(=O)C>O>[F:26][CH:2]([F:1])[C:3]([CH3:24])([CH3:25])[CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([NH:14][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:8]=1参加物
実験手順
1,1-Difluoro-2,2-dimethyl-3-[3-(N-phenyl-N-acetylamino)-4fluorobenzyloxy]propane (0.5 g) was suspended in a 1 molar solution of potassium hydroxide in water containing 20% by volume ethanol and the mixture was heated at the reflux temperature for 8 hours. After standing overnight at the ambient temperature, the mixture was shaken several times with ethyl acetate and the combined organic extracts washed with water and brine, and dried over anhydrous magnesium sulphate. Evaporation of the solvent under reduced pressure gave a brown oil which was purified by column chromatography on a silica gel supoort, eluting with petroleum ether (boiling range 40°-60° C.) containing 10% by volume ethyl acetate, to give the title compound (0.23 g) as a pale yellow oil.
後処理
- temperaturethe mixture was heated at the reflux temperature for 8 hours
- washthe combined organic extracts washed with water and brine
- dry with materialdried over anhydrous magnesium sulphate
- customEvaporation of the solvent under reduced pressure
- customgave a brown oil which
- customwas purified by column chromatography on a silica gel supoort
- washeluting with petroleum ether (boiling range 40°-60° C.)
- additioncontaining 10% by volume ethyl acetate
出典と根拠
- ORDレコード
- ord-a97baa1ff93c429eb52f47454fbbfa89
- 出典データセット
- uspto-grants-1988_12
- 特許番号
- US04792563
関連ノート
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