反应详情

0.8 g of 2-tert-Butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclobutyl-pyrimidine (2.28 mmol), 0.29 g of 4-methyl-3-mercapto-1,2,4-triazole (2.52 mmol), 0.15 g of lithium hydroxide and a tip of a spatula of potassium iodide were dissolved in 20 ml of dimethylformamide. The mixture was stirred for 14 h at room temperature and then extracted with water and ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and evaporated to dryness. The residue was then purified by column chromatography on silica gel (dichloromethane-methanol (2-10%)) to yield an oily residue that was precipitated with acetonitrile thereby yielding 0.46 g of the title compound (47%).

1. extractionextracted with water and ethyl acetate
2. dry with materialThe organic layer was dried over magnesium sulfate
3. filtrationfiltered
4. customevaporated to dryness
5. customThe residue was then purified by column chromatography on silica gel (dichloromethane-methanol (2-10%))
6. customto yield an oily residue that
7. customwas precipitated with acetonitrile