反应详情

0.39 g (0.0022 mol) of (4,6-dichloro-pyrimidin-2-yl)methylamine and 1.1 g (0.0044 mol) of 4-tert-butyl-benzenesulfonamide potassium salt were stirred in 10 ml of 1-methyl-2-pyrrolidone at 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, de-gassed in a vacuum and made acid with 4N HCl, with a precipitate separating. The mixture was suction 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 0.57 g (73%) of 4-tert-butyl-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide as white crystals; m.p.: 118-137° C. (dec.).

1. distillationThen, the solvent was distilled off in a high vacuum
2. customthe residue was partitioned in ethyl acetate/water
3. extractionextracted
4. customde-gassed in a vacuum
5. customwith a precipitate separating
6. filtrationfiltered
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