反应详情

Into a 2 l three-neck flask were added compound (F) (25 g, 0.109 mol) obtained in the fifth step and ethylene glycol (722 ml) and further an aqueous solution obtained by dissolving KOH (18.8 g, 0.335 mol) in water (26 ml), followed by refluxing the mixture for 12 hours while heating on a mantle heater. After cooling, the reaction mixture was acidified by adding 6N-HCl (200 ml) to form crystals, which were filtered off and dried, followed by dissolving the crystals in ethanol (200 ml) and recrystallizing to obtain 4-(trans-4'-methyloxymethylcyclohexyl)benzoic acid (G) (18.8 g). This had a melting point (C-N point) of 132.7° C. and a clearing point (N-I point) of 234.6° C.

1. customfurther an aqueous solution obtained
2. temperatureby refluxing the mixture for 12 hours
3. temperaturewhile heating on a mantle heater
4. temperatureAfter cooling
5. customto form crystals, which
6. filtrationwere filtered off
7. customdried
8. dissolutionby dissolving the crystals in ethanol (200 ml)
9. customrecrystallizing