Hydrochloric Acid → N-(6-chloro-2-(2-cyanopyridin-4-yl)-5-(2-methoxyphenoxy)pyrimidin-4-yl)-5-isopropylpyridine-2-sulfonamide

温度

40 °C

8.95 g (24 mmol) of 4-[4,6-dichloro-5-(2-methoxy-phenoxy)-pyrimidine-2-yl]-pyridine-2-carbonitrile were suspended in 100 ml of acetone. At a temperature of 20° C., 5.04 g (25 mmol) of 5-isopropyl-pyridine-2-sulfonamide, 1 ml of de-ionized water, 10.6 g (77 mmol) of potassium carbonate and 135 mg (1.2 mmol) 1,4-diazobicyclo[2.2.2]octane were added. The mixture was stirred at 40° C. for 20 hr. Thereafter, another 240 mg (1.2 mmol) of 5-isopropyl-pyridine-2-sulfonamide and 80 mg (0.7 mmol) of 1,4-diazobicyclo[2.2.2]octane were added. The reaction mixture was stirred for 24 hr at 40° C. followed by cooling to 20° C. Then 50 ml of de-ionized water and 45 ml of 3 N aqueous hydrochloric acid were added slowly until pH=1. The acetone was removed by distillation and the resulting suspension was stirred at 20° C. for 1.5 hr. The solid was filtered off under suction, washed first with 100 ml of de-ionized water and thereafter with 50 ml of t-butylmethylether. Then the solid was dried at 70° C., 2000 Pa for 20 hr. There were obtained 13.2 g (102% of theory) of 5-isopropyl-pyridin 2-sulfonic acid [6-chloro-2-(2-cyano-pyridine-4-yl)-5-(2-methoxy-phenoxy)-pyrimidine-4-yl]-amide with a HPLC purity of 87.8% (w/w).

1. stirringThe reaction mixture was stirred for 24 hr at 40° C.
2. temperatureby cooling to 20° C
3. customThe acetone was removed by distillation
4. stirringthe resulting suspension was stirred at 20° C. for 1.5 hr
5. filtrationThe solid was filtered off under suction
6. washwashed first with 100 ml of de-ionized water
7. customThen the solid was dried at 70° C.
8. wait2000 Pa for 20 hr

ORDレコード

ord-a5829e667dba467d91941ec1aa1c7743

出典データセット

uspto-grants-2000_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06103902