反应详情

0.46 g (0.0026 mol) of (4,6-dichloro-pyrimidin-2-yl)-methylamine and 1.1 g (0.0051 mol) of 4-fluoro-benzenesulfonamide potassium salt were stirred in 10 ml of 1-methyl-2-pyrrolidone in 150° C. for 8 hours. Then, the solvent was distilled off in a high vacuum, the residue was partitioned in ethyl acetate/water and extracted. The aqueous phase was saturated with sodium chloride, evaporated briefly in a vacuum and made acid with 4N HCl, with a precipitate separating. The mixture was suctioned filtered, the extract and the solid were combined and chromatographed over silica gel with cyclohexane/ethyl acetate 2:1 as the eluent. The product was recrystallized from ethyl acetate/n-hexane. There was obtained 0.46 g (56%) of N-(6-chloro-2-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide as white crystals; m.p. 121-123 C.

1. distillationThen, the solvent was distilled off in a high vacuum
2. customthe residue was partitioned in ethyl acetate/water
3. extractionextracted
4. customevaporated briefly in a vacuum
5. customwith a precipitate separating
6. filtrationThe mixture was suctioned filtered
7. extractionthe extract
8. customchromatographed over silica gel with cyclohexane/ethyl acetate 2:1 as the eluent
9. customThe product was recrystallized from ethyl acetate/n-hexane