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), 0.35 g of 4-Methyl-4H-[1,2,4]triazole-3-thiol (3.04 mmol), 0.2 g of lithium-hydroxide (8.35 mmol) and a spatula tip of potassium iodide werde stirred for 72 h in 20 ml of dimethylformamide. Water and ethyl acetate were added and the organic layer was separated, dried over magnesium sulfate, filtered and the solvent was evaporated. The resdue was subjected to a column chromatography on silica gel using dichloromethane-methanol(2-10%). Fractions containing the product were combined, the solvent was evaporated and the residue re-dissolved in isopropanol. The solution was treated with HCl/isopropanol. Diisopropylethylether was added whereby an oily precipitate formed. The solvent was decanted and the remaining oil evaporated to dryness to yield 1.1 g (77%) of the title compound as a white solid.

1. customthe organic layer was separated
2. dry with materialdried over magnesium sulfate
3. filtrationfiltered
4. customthe solvent was evaporated
5. additionFractions containing the product
6. customthe solvent was evaporated
7. dissolutionthe residue re-dissolved in isopropanol
8. additionThe solution was treated with HCl/isopropanol
9. additionDiisopropylethylether was added whereby an oily precipitate
10. customformed
11. customThe solvent was decanted
12. customthe remaining oil evaporated to dryness