反应详情

A mixture of 3'-bromo-4'-(2-methylbutyloxy)-4-biphenylylbenzoate (4.8 g) from step (IV), a 40% aqueous solution (3.2 g) of NaOH and ethanol (100 ml) was heated under reflux for 3 hours, followed by distilling off ethanol, adding toluene, acidifying with 6N hydrochloric acid, heating to dissolve insolubles, separating the solution layer, washing with water, further washing with an aqueous solution of sodium hydrogen sulfite, washing with water to make the solution neutral, drying, distilling off toluene and recrystallizing the residue from n-heptane to obtain 3'-bromo-4'-(2-methylbutyloxy)-4-hydroxybiphenyl (3.0 g). M.p.: 75°~76.5° C.

1. temperatureunder reflux for 3 hours
2. distillationby distilling off ethanol
3. additionadding toluene
4. temperatureheating
5. dissolutionto dissolve insolubles
6. customseparating the solution layer
7. washwashing with water
8. washfurther washing with an aqueous solution of sodium hydrogen sulfite
9. washwashing with water
10. customdrying
11. distillationdistilling off toluene
12. customrecrystallizing the residue from n-heptane