Thionyl Chloride → 4-(Chlorocarbonyl)phenyl benzoate
反応式
[C:1]([O:9][C:10]1[CH:18]=[CH:17][C:13]([C:14](O)=[O:15])=[CH:12][CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:21])=O>CN(C)C=O>[C:1]([O:9][C:10]1[CH:18]=[CH:17][C:13]([C:14]([Cl:21])=[O:15])=[CH:12][CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
10.00 g (41.3 mmol) of 4-(benzoyloxy)benzoic acid and one drop of N,N-dimethylformamide are refluxed in 40 ml of thionyl chloride with stirring until gas is no longer evolved. The excess thionyl chloride is very substantially removed by distillation under reduced pressure and co-distilled twice with petroleum ether (50/70) under reduced pressure from the remaining residue for complete removal. Purification is carried out by recrystallization from 150 ml of petroleum ether (50/70)/ethyl acetate 2:1, and the crystals are washed with 4 ml of petroleum ether (50/70)