p-Toluenesulfonic acid → HCID 14071800、化合物
反応式
[Cl:1][C:2]1[C:20]([Cl:21])=[C:19]([F:22])[C:18]([F:23])=[CH:17][C:3]=1[C:4]([CH:6](C(OCC)=O)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].C1(C)C=CC(S(O)(=O)=O)=CC=1>O>[Cl:1][C:2]1[C:20]([Cl:21])=[C:19]([F:22])[C:18]([F:23])=[CH:17][C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]参加物
4
実験手順
To an emulsion of diethyl 2-(2,3-dichloro-4,5-difluorobenzoyl)malonate (9.71 g) in water (11.2 ml) was added p-toluenesulfonic acid (11.2 mg) and refluxed for 3 hours with stirring vigorously. After cooling, the reaction mixture was extracted with dichloromethane. The organic layer was washed with 7% aqueous sodium carbonate solution and then with water successively, dried over anhydrous sodium sulfate and concentrated. The residue was recrystallized from n-hexane to give the title compound (4.24 g) as powdery crystals. mp 52°-53° C.