[Cl-].BrBr.[Cl:4][CH:5]1[CH:13]=[CH:12][CH:8]([C:9]([Cl:11])=[O:10])[CH:7]([C:14]([Cl:16])=[O:15])[CH2:6]1>ClC1C=CC=CC=1>[Cl:4][C:5]1[CH:6]=[C:7]([C:14]([Cl:16])=[O:15])[C:8](=[CH:12][CH:13]=1)[C:9]([Cl:11])=[O:10]To a 1-l three-necked flask, equipped with a mechanical stirrer, a condenser with a gas outlet and an equa-pressured addition funnel, is charged 241.5 g (1 mole) of 4-chloratetrahydrophthaloyl chloride and 36 g of chlorobenzene. The mixture is heated to 100°-110° C. with stirring. Bromine, 320 g (2 moles) is added dropwise into the solution in a sub-surface manner. The color dissipates quickly and an evolution of gas occurs. When approximately 240 g of bromine has been added, the pot temperature is raised to 135° C. The addition of bromine continues until completion. The pot temperature is then raised to 165°-170° C. for 2-4 fours. during this period, an additional amount of bromine, such as about 10 to 15 g, may be added to complete the conversion of 4-chlorotetrahydrophthaloyl chloride. A good yield of 4-chlorophthaloyl chloride will be obtained from the distillation of the mixture.
Wird geladen…
