反应详情

First, 43.7 g of 3,5-dibromo-1H-1,2,4-triazole is introduced into 200 mL of tetrahydrofuran (THF), the resultant mixture is agitated, and 40.4 g of 2-chloro-2,4-difluoroacetophenone is further introduced thereto. Next, 36.3 g of potassium carbonate is introduced to the reaction mixture and the resultant mixture is agitated for 7 hours at room temperature. After the completion of the reaction, the reaction mixture is filtered, washed with 100 mL of tetrahydrofuran (THF), and concentrated at room temperature. Then, 437 mL of purified water is introduced so that the crystals are slurried, followed by filtering. The filtered crystals are reslurried in 175 mL of isopropanol and filtered again. The crystals are washed with 44 mL of isopropanol and dried with hot air at 50° C. to obtain 63.8 g of the title compound as a white solid (yield 87%, purity 99.2%, HPLC, detected at a wavelength of 256 nm, 18C 4.6×250 mm, mobile phase 60% ACN, flow rate 1 mL/min).

1. customAfter the completion of the reaction
2. filtrationthe reaction mixture is filtered
3. washwashed with 100 mL of tetrahydrofuran (THF)
4. concentrationconcentrated at room temperature
5. additionThen, 437 mL of purified water is introduced so that the crystals
6. filtrationby filtering
7. filtrationfiltered again
8. washThe crystals are washed with 44 mL of isopropanol
9. customdried with hot air at 50° C.