反应详情

温度

20 °C

12.5 g (33.5 mmol) of 4-[4,6-dichloro-5-(2-methoxy-phenoxy)-pyrimidine-2-yl]-pyridine-2-carbonitrile and 6.06 g (35 mmol) of 5-methyl-pyridine-2-sulfonamide were added to 130 ml of acetone. 15 g of potassium carbonate and 190 mg (1.6 mmol) of 1,4-diazobicyclo[2.2.2]octane were added and the suspension was stirred at 40° C. for 5 hr and at 20° C. for 15 hr. Then 50 ml of de-ionized water were added followed by dropwise addition of 50 ml of 3 N hydrochloric acid (pH of the solution=1). Acetone was removed by evaporation and the suspension was stirred for 1 hr. The solid was filtered and washed with 100 ml of water. The residue was heated (reflux) in 100 ml of methanol for 1 hr followed by cooling to 20° C. The solid was filtered and dried at 80° C., 2000 Pa for 16 hr. There were obtained 16.0 g (93% of theory) of 5-methyl-pyridine-2-sulfonic acid [6-chloro-2-(2-cyano-pyridine-4-yl)-5-(2-methoxy-phenoxy)-pyrimidine-4-yl]-amide with a HPLC purity of 90.3% (w/w).

1. customAcetone was removed by evaporation
2. stirringthe suspension was stirred for 1 hr
3. filtrationThe solid was filtered
4. washwashed with 100 ml of water
5. temperatureThe residue was heated
6. temperature(reflux) in 100 ml of methanol for 1 hr
7. temperatureby cooling to 20° C
8. filtrationThe solid was filtered
9. customdried at 80° C.
10. wait2000 Pa for 16 hr