反应详情

0.58 g (0.00266 mol) of 4,6-dichloro-2-pyrrolidin-1-yl-pyrimidine and 1.36 g (0.00539 mol) of N-(4-sulfamoyl-phenyl) -acetamide potassium salt were stirred in 10 ml of 1-methyl-2-pyrrolidone at 140° 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 ethyl acetate. Both organic phases were combined and concentrated. The residue was recrystallized from a small amount of ethanol and the mother liquor was chromatographed over silica gel with cyclohexane/ethyl acetate 2:1 as the eluent. There was obtained a total of 0.62 g (66%) of N-[4-(6-chloro-2-pyrrolidin-1-yl-pyrimidin-4-ylsulfamoyl)-phenyl]-acetamide as whitish crystals; m.p. 229-233° C.

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 ethyl acetate
5. concentrationconcentrated
6. customThe residue was recrystallized from a small amount of ethanol
7. customthe mother liquor was chromatographed over silica gel with cyclohexane/ethyl acetate 2:1 as the eluent