Hydrochloric Acid → HCID 58335273、化合物
反応式
C([O:3][CH:4](OCC)[C:5]1[CH:10]=[CH:9][C:8]([C:11]([OH:14])([CH3:13])[CH3:12])=[CH:7][C:6]=1[F:15])C.Cl>CC(C)=O>[F:15][C:6]1[CH:7]=[C:8]([C:11]([OH:14])([CH3:12])[CH3:13])[CH:9]=[CH:10][C:5]=1[CH:4]=[O:3]参加物
4
実験手順
A solution of 2-[4-(diethoxymethyl)-3-fluorophenyl]propan-2-ol (25.6 g, 100 mmol) in acetone (50 mL) was added dropwise to aqueous HCl (6M, 50 mL) cooled with ice-water to keep the internal temperature less than 10° C. After addition, the mixture was stirred at room temperature for 6 hrs. The mixture was extracted twice with ethyl acetate. The combined organics were washed with saturated aqueous sodium bicarbonate and brine, dried over sodium sulfate and concentrated to afford the title compound. 1H NMR (300 MHz, CDCl3): δ 10.23 (s, 1H), 7.81 (d, 1H), 7.34 (d, 1H), 7.30 (d, 1H), 2.01 (s, 1H), 1.49 (s, 61-1).
後処理
- customthe internal temperature less than 10° C
- additionAfter addition
- extractionThe mixture was extracted twice with ethyl acetate
- washThe combined organics were washed with saturated aqueous sodium bicarbonate and brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-b333625433eb43ddbb75f1cc72048106
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08278335B2
反応ノート
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