反应详情

温度

60 °C

To a solution of 3-fluoro-4-cyanophenol (1.5 g, 11 mmols) dissolved in dry pyridine (5 cc) was added a solution of 4-(β-ethoxyethoxy)benzoic acid chloride (2.5 g, 11 mmols) dissolved in dry toluene (10 cc), followed by heating the mixture with stirring at 60° C. for 3 hours, thereafter adding it to water (100 cc), washing the resulting separated toluene layer with 6N-hydrochloric acid, 2N-NaOH aqueous solution and water, in this order, drying over anhydrous sodium sulfate, distilling off toluene from the toluene layer and recrystallizing the resulting oily residue from ethyl alcohol (10 cc) to obtain the objective 3-fluoro-4-cyanophenyl 4-(β-ethoxyethoxy)benzoate (2.1 g) (yield: 64%).

1. temperatureby heating the mixture
2. washwashing the resulting
3. customseparated toluene layer with 6N-hydrochloric acid, 2N-NaOH aqueous solution and water
4. dry with materialin this order, drying over anhydrous sodium sulfate
5. distillationdistilling off toluene from the toluene layer
6. customrecrystallizing the resulting oily residue from ethyl alcohol (10 cc)