反应详情

温度

5 °C

To a 22 L open-mouth round bottom flask fitted with a three-necked flange head, a mechanical stirrer, a nitrogen inlet and an outlet connected to a HCl scrubbing tower was added 2,5-dichlorobenzoic chloride (4500 g, 21.5 mol) and phenyl ether (5489 g, 32.3 mol). The solution was cooled in ice to 5° C. under stirring and aluminum chloride (3700 g, 7.8 mol) was added slowly. After about 300 g aluminum chloride was added, the solution started to foam violently. The rest was added carefully over about 10 min. On several occasions, the stirring had to be stopped to control the foaming. The temperature of the reaction mixture was about 35° C. after the addition. The mixture was then stirred for about 30 min. and poured into about 20 gallon of ice water. The large reddish mass was dissolved by adding about 12 L of methylene chloride and stirring. The organic layer was separated and the aqueous layer was extracted with some methylene chloride. After methylene chloride was removed from the combined organic layer by distillation, the residue was recrystallized twice from cyclohexane (2×10 L), washed with cooled hexane, air dried and then vacuum dried to afford 5387 g monomer (73%). The mother liquor was kept for later recovery of remaining product.

1. customTo a 22 L open-mouth round bottom flask fitted with a three-necked flange head, a mechanical stirrer, a nitrogen inlet and an outlet
2. additionThe rest was added carefully over about 10 min
3. customwas about 35° C.
4. additionafter the addition
5. stirringThe mixture was then stirred for about 30 min.
6. dissolutionThe large reddish mass was dissolved
7. stirringstirring
8. customThe organic layer was separated
9. extractionthe aqueous layer was extracted with some methylene chloride
10. customAfter methylene chloride was removed from the combined organic layer by distillation
11. customthe residue was recrystallized twice from cyclohexane (2×10 L)
12. washwashed with cooled hexane, air
13. customdried
14. customvacuum dried