反应详情

温度

80 °C

To a 22 L, three-necked flask fitted with a thermometer, mechanical stirrer and a Vigreux column connected to an aqueous NaOH scrubbing tower, was added 1,4-dichlorobenzene (3 Kg, 26.4 mol) and benzoyl chloride (2.6 Kg, 18.55 mol). The mixture was heated to 80° C. to give a homogeneous solution. Aluminum chloride (5.5 Kg, 41.25 mol) was added over 12 min. with stirring. (The molar ratio of reactants was 2.2:1.4:1.0 (AlCl3 : Dichlorobenzene:Benzoyl Chloride)). The resulting mixture was heated to 140° C. over 60 min followed by heating to 175° C. over 30 min. Heating was stopped at 175° C. The mixture was allowed to cool to 80° C. over two hours and poured into a well stirred mixture of ice and water (ca. 25 L water and 15 Kg of ice) over 30 min. The organic solid was collected by filtration and dissolved in 7 L of toluene. The solution was washed with aqueous sodium bicarbonate and dried. Toluene was removed by distillation. Pure 2,5-dichlorobenzophenone was isolated in 80% yield after recrystallization from hexane and toluene. Gas chromatography indicated an absolute yield of 97%.

1. customTo a 22 L, three-necked flask fitted with a thermometer, mechanical stirrer
2. customto give a homogeneous solution
3. temperatureThe resulting mixture was heated to 140° C. over 60 min
4. temperatureby heating to 175° C. over 30 min
5. temperatureHeating
6. customwas stopped at 175° C
7. temperatureto cool to 80° C. over two hours
8. additionpoured into a well
9. stirringstirred
10. filtrationThe organic solid was collected by filtration
11. dissolutiondissolved in 7 L of toluene
12. washThe solution was washed with aqueous sodium bicarbonate
13. customdried
14. customToluene was removed by distillation