HCID 57799869、化合物 → HCID 57799540、化合物
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:13][CH2:14][C:15]([OH:17])=O)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][O:11][CH3:12]>O=S(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]2[C:5](=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][O:11][CH3:12])[C:15](=[O:17])[CH2:14][CH2:13]2参加物
3
反応条件
- 温度
- 45 °C
実験手順
The mixture of 3-[3-Fluoro-4-(2-methoxy-ethoxy)-phenyl]-propionic acid (16 g) in SOCl2 (50 ml) was refluxed for 4 hours. The mixture was evaporated, the residue was dissolved in CS2 (100 ml), and then AlCl3 (20 g) was added. The mixture was heated at 45° C. for 4 hours. 200 ml of ice-water was added to the cooled mixture and the mixture was stirred for another 1 hour. The mixture was extracted by ethyl acetate (300 ml×3). The product was purified by flash column chromatography using ethyl acetate:PE=5:1 as eluent. LC-MS: m/e 225 (MH+).
後処理
- temperaturewas refluxed for 4 hours