反应详情

0.2 g of the compound obtained in Example 38 in 3.5 ml of POCl3 was stirred with 0.083 g of PCl5 at 20° C. for 2 hours. Thereafter, the POCl3 was distilled off and the residue was partitioned between ethyl acetate and aqueous sodium bicarbonate (sic). The organic phase was washed with water, dried and the solvent was evaporated. The residue was chromatographed over silica gel with chloroform-methanol, thereafter recrystallized from dichloromethane-ethanol. 0.150 g of 5-isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-chloromethyl-2-morpholin-4-yl-pyrimidin-4-ylamide, m.p. 205° C., was obtained.

1. distillationThereafter, the POCl3 was distilled off
2. customthe residue was partitioned between ethyl acetate and aqueous sodium bicarbonate (sic)
3. washThe organic phase was washed with water
4. customdried
5. customthe solvent was evaporated
6. customThe residue was chromatographed over silica gel with chloroform-methanol
7. customrecrystallized from dichloromethane-ethanol