反应详情

0.24 g (0.00135 mol) of (4,6-dichloro-pyrimidin-2-yl)-methylamine and 0.62 g (0.0027 mol) of 3-chloro-benzene-sulfonamide 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 made acid with 4N HCl and extracted with dichloromethane. The residue was chromatographed over silica gel with cyclohexane/ethyl acetate 2:1 as the eluent. There was obtained 0.24 g (53%) of 3-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide as yellow crystals; m.p. 120-130° 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. extractionextracted with dichloromethane
5. customThe residue was chromatographed over silica gel with cyclohexane/ethyl acetate 2:1 as the eluent