反应详情

温度

160 °C

Anhydrous p-toluene sulfonic acid (10 g, 52.57 mmol) was melted at 120° C. and 3-amino-4-methoxy benzoic acid methyl ester (3.88 g, 21.44 mmol) obtained in step 1 of Preparation Example 1 and 3-chloro-4-fluorobenzonitrile (5.0 g, 32.14 mol) were added thereto and stirred at 160° C. for 8 hours. The resulting solution was cooled to room temperature and the reaction was stopped by adding NaHCO3 thereto. The resulting mixture was 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 (3.24 g, 9.62 mmol) in a yield of 45%.

1. additionwere added
2. temperatureThe resulting solution was cooled to room temperature
3. extractionThe resulting mixture was extracted with ethyl acetate
4. dry with materialthe extract was dried over MgSO4
5. concentrationconcentrated under a reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography