反应详情

To a solution of 2-methoxy-4-(trifluoromethyl)benzonitrile (Description 94; 19 g, 94.4 mmol) in ethanol (150 ml) was added a solution of potassium hydroxide (26.43 g; 472 mmol) in water (100 ml) and the resulting mixture heated at reflux overnight. The mixture was cooled and the ethanol removed by evaporation, the remaining aqueous phase was extracted with diethyl ether then acidified with 5N HCl. The acidic aqueous phase was then extracted with EtOAc (3×200 ml) and the combined organic layers washed with water, sat NaCl, dried over Na2SO4, filtered and evaporated to give the title compound (19.91 g, 95%).

1. temperaturethe resulting mixture heated
2. temperatureat reflux overnight
3. temperatureThe mixture was cooled
4. customthe ethanol removed by evaporation
5. extractionthe remaining aqueous phase was extracted with diethyl ether
6. extractionThe acidic aqueous phase was then extracted with EtOAc (3×200 ml)
7. washthe combined organic layers washed with water
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. customevaporated