反应详情

4-n-Octyloxy-4'-acetylbiphenyl (38.5 g, 0.119 mol), formic acid (23.8 g, 5.17 mols) and toluene (200 ml) were heated to 60° C., followed by dropwise adding a 35% H2O2 aqueous solution (160.7 g, 1.04 mol) over 1.5 hour while keeping the liquid temperature at 70°~75° C., thereafter heating at 60°~70° C. for 3 hours with stirring, cooling down to room temperature, extracting with toluene (1.5 l), washing with water till the washing water became neutral, drying, removing toluene, adding ethanol (200 ml), heating under reflux, somewhat cooling, adding a 40% NaOH aqueous solution (80 ml ), again heating under reflux for 2 hours, pouring the solution in 6N hydrochloric acid (1 l), stirring, collecting the resulting solids by suction filtering, adding toluene (300 ml), withdrawing water and recrystallizing to obtain 4-hydroxy-4'-n-octyloxybiphenyl (18.5 g). Yield: 50.6%. M.P.: 153.6° C.

1. customat 70°~75° C.
2. temperatureheating at 60°~70° C. for 3 hours
3. extractionextracting with toluene (1.5 l)
4. washwashing with water till the washing water
5. customdrying
6. customremoving toluene
7. additionadding ethanol (200 ml)
8. temperatureheating
9. temperatureunder reflux
10. temperaturesomewhat cooling
11. additionadding a 40% NaOH aqueous solution (80 ml )
12. temperatureagain heating
13. temperatureunder reflux for 2 hours
14. additionpouring the solution in 6N hydrochloric acid (1 l)
15. stirringstirring
16. customcollecting the resulting solids by suction
17. filtrationfiltering
18. additionadding toluene (300 ml)
19. customwithdrawing water
20. customrecrystallizing