Thionyl Chloride → HCID 19783302、化合物
反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH:9](O)[CH:10]([C:12]1[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=1)[CH3:11].S(Cl)(Cl)=O>>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8]/[CH:9]=[C:10](\[C:12]1[CH:13]=[CH:14][N:15]=[CH:16][CH:17]=1)/[CH3:11]参加物
3
反応条件
- 温度
- 40 °C
実験手順
To the said solid, that is, 1.59 g (6.49 mmol) of 1-(2-fluorophenyl)-3-(4-pyridyl)-2-butanol, 2.5 ml of thionyl chloride was added and stirred for one hour at 40° C. After distilling away excessive thionyl chloride under reduced pressure, water was added and the residue was alkalized with sodium carbonate and was extracted with ethyl acetate. After drying over anhydrous sodium sulfate, ethyl acetate was distilled away under reduced pressure to obtain a brown oily substance. The resulting oily substance was purified by silica gel column chromatography to obtain 0.54 g of the desired compound (yield: 31.6%).
後処理
- distillation