反应详情

0.4 g of 2-tert-Butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclobutyl-pyrimidine (1.14 mmol), 0.2 g of 4-methyl-5-cyclopropyl-4H-[1,2,4]triazole-3-thiol (1.29 mmol), 0.07 g lithium-hydroxide (2.92 mmol) and a spatula tip of potassium iodide were stirred in 20 ml of dimethylformamide overnight at room temperature and for an additional 3 h at 40° C. After addition of water and ethyl acetate, the organic layer was separated, dried over magnesium sulfate, filtered and the solvent was evaporated. The residue was purified by column chromatography on silica gel using dichloromethane-methanol (0-2%). Fractions containing the product were combined and the solvents were evaporated. The residue was dissolved in isopropanol and 1 equivalent of fumaric acid was added. The solvent was evaporated and the residue was dissolved in diisopropylether to which some drops of isopropanol were added upon warming, thereby forming a precipitate. After cooling the precipitate was collected by filtration and dried. Yield: 0.04 g (6%)

1. customthe organic layer was separated
2. dry with materialdried over magnesium sulfate
3. filtrationfiltered
4. customthe solvent was evaporated
5. customThe residue was purified by column chromatography on silica gel
6. additionFractions containing the product
7. customthe solvents were evaporated
8. dissolutionThe residue was dissolved in isopropanol
9. customThe solvent was evaporated
10. dissolutionthe residue was dissolved in diisopropylether to which some drops of isopropanol
11. additionwere added
12. temperatureupon warming
13. customforming a precipitate
14. temperatureAfter cooling the precipitate
15. filtrationwas collected by filtration
16. customdried