反应详情

温度

100 °C

o-Allylphenol (52.2 g), 4,4'-difluorobenzophenone (35 g), 4-fluorobenzophenone (13.8 g), potassium carbonate (37.75 g), dry N-methylpyrrolidone (200 ml) and toluene (75 ml) are placed in a 3-necked 1500 ml flask fitted with a stirrer, reflex condensor and thermometer and the mixture is heated under nitrogen to a temperature between 155°-160° C. and stirred for 3 hours. Water and toluene are separated via a Dean Stark trap and finally after 3 hours the reaction mixture reaches a temperature of 160° C. The mixture is cooled to 100° C. and a 1:1 mixture of toluene/water (400 ml) is added while stirring. After phase separation the aqueous layer is washed with toluene (100 ml) and the combined toluene layers are washed 4 times with water (150 ml). The toluene phase is dried over sodium sulphate and toluene distilled off by use of a rotary evaporator finally in vacuum leaving a 4,4'-bis[o-(1-propenyl)phenoxy]benzophenone/4-[o-(1-propenyl)phenoxy]benzophenone mixture as a light yellow melt. The yield is 89 g.

1. customfitted with a stirrer
2. temperaturereflex condensor and thermometer and the mixture is heated under nitrogen to a temperature between 155°-160° C.
3. customWater and toluene are separated via a Dean Stark trap and finally after 3 hours the reaction mixture
4. customa temperature of 160° C
5. additiona 1:1 mixture of toluene/water (400 ml)
6. additionis added
7. stirringwhile stirring
8. customAfter phase separation the aqueous layer
9. washis washed with toluene (100 ml)
10. washthe combined toluene layers are washed 4 times with water (150 ml)
11. dry with materialThe toluene phase is dried over sodium sulphate and toluene
12. distillationdistilled off by use of a rotary evaporator finally in vacuum