反应详情

温度

65 °C

DMSO (300 ml) and KOH (38.0 g) were added to 1,1-bis(4-hydroxyphenyl)-4-(trans-4-n-propylcyclohexyl)cyclohexane (110.6 g) obtained in the first step, followed by dissolving these together on heating to 65° C., dropwise adding to the solution, a solution of p-chloronitrobenzene (97.8 g) in DMSO (500 ml) at 65° C., reacting the mixture, aging for 5 hours, cooling down to room temperature after completion of the reaction, extracting with dichloromethane, washing with lN-NaOH aqueous solution and further with saturated NaCl aqueous solution till the aqueous solution became neutral, drying over MgSO4, treating by alumina column, distilling off the resulting eluate and recrystallizing the resulting concentrate from a mixed solvent of toluene-acetone to obtain pale yellow crystals of 1,1-bis[4-(4-nitrophenoxy)phenyl]-4-(trans-4-n-propylcyclohexyl)cyclohexane (136.1 g).

1. customobtained in the first step
2. dissolutionby dissolving these together
3. additiondropwise adding to the solution
4. customat 65° C.
5. temperaturecooling down to room temperature
6. customafter completion of the reaction
7. extractionextracting with dichloromethane
8. washwashing with lN-NaOH aqueous solution
9. dry with materialdrying over MgSO4
10. additiontreating by alumina column
11. distillationdistilling off the resulting eluate and
12. customrecrystallizing the resulting
13. concentrationconcentrate from a mixed solvent of toluene-acetone