反应详情

1 g of 2-tert-Butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-tert-butyl-pyrimidine (2.83 mmol), 0.4 g of 4-Methyl-5-methyl-4H-[1,2,4]triazole-3-thiol (3.09 mmol), 0.2 g of lithium-hydroxide (8.35 mmol) and a spatula tip of potassium iodide werde stirred in 20 ml of dimethylformamide for 2 h at 80° C. After addition of water and ethyl acetate, the organic phase was separated and dried over magnesium sulfate. After filtration and evaporation of the solvent, the crude product was purified by column chromatography on silica gel using dichloromethane-methanol (1-6%). Fractions containing the product were combined and the solvent was evaporated. The residue was dissolved in isopropanol, and a solution of HCl in isopropanol was added. On addition of diisopropylethylether, the product formed an oily mass. The solvent was decanted and the remaining oil evaporated to dryness to yield 0.6 g (41%) of the title compound as a white solid.

1. customthe organic phase was separated
2. dry with materialdried over magnesium sulfate
3. filtrationAfter filtration and evaporation of the solvent
4. customthe crude product was purified by column chromatography on silica gel
5. additionFractions containing the product
6. customthe solvent was evaporated
7. dissolutionThe residue was dissolved in isopropanol
8. additiona solution of HCl in isopropanol was added
9. additionOn addition of diisopropylethylether
10. customthe product formed an oily mass
11. customThe solvent was decanted
12. customthe remaining oil evaporated to dryness