反应详情

温度

160 °C

Anhydrous p-toluenesulfonic acid (6.30 g, 33.1 mmol) was added to 50 ml of benzene and the resulting mixture was refluxed while removing water using a dean-stock trap. Added thereto were 3-amino-4-methoxy benzoic acid methyl ester (3 g, 16.6 mmol) obtained in step 1 of Preparation Example 1 and 4-nitrobenzonitrile (2.94 g, 19.9 mol), followed by stirring at 160° C. for 8 hours. The resulting solution was cooled to room temperature, the reaction was stopped by adding NaHCO3 thereto, extracted with ethyl acetate, the extract was dried over MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (2.83 g, 8.59 mmol) in a yield of 52%.

1. temperaturethe resulting mixture was refluxed
2. customwhile removing water using a dean-stock trap
3. additionAdded
4. temperatureThe resulting solution was cooled to room temperature
5. extractionextracted with ethyl acetate
6. dry with materialthe extract was dried over MgSO4
7. concentrationconcentrated under a reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography