反应详情

温度

140 °C

To a stirred round bottled flask with toluene (100 mL) ethyl benzoyl acetate (18.7 g, 97 mmol) and m-anisidine (12 g, 97 mmol) was added. 4 M HCl in dioxane (0.5 mL) was added and the reaction mixture was refluxed for 6 h (140° C.). The mixture was co-evaporated with toluene. To the crude mixture diphenyl ether (50 mL) was added and the mixture was heated to 280° C. for 2 h. When the theoretical amount ethanol (6 mL) was collected in a Dean Stark trap the heating was stopped and the mixture was cooled to rt. The crude mixture was dissolved in CH2Cl2 (100 mL) and stirred for 30 min. The formed precipitate was filtered off and dried which gave 1 (4.12 g, 16.4 mmol, 17%): pale yellow powder.

1. additionwas added
2. temperaturethe mixture was heated to 280° C. for 2 h
3. customWhen the theoretical amount ethanol (6 mL) was collected in a Dean Stark trap the heating
4. temperaturethe mixture was cooled to rt
5. dissolutionThe crude mixture was dissolved in CH2Cl2 (100 mL)
6. filtrationThe formed precipitate was filtered off
7. customdried which