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), 0.22 g of 4-methyl-5-trifluoromethyl-4H-[1,2,4]triazole-3-thiol (1.2 mmol), 0.07 g of lithium-hydroxide (2.92 mmol) and a spatula tip of potassium iodide were stirred in 10 ml of dimethylformamide for 14 h at room temperature and for an additional 2 h at 80° 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 twice by column chromatography on silica gel using dichloromethane-methanol (1-5%). Fractions containing the product were combined, the solvents evaporated, the residue stirred with acetonitrile yielding 0.03 g (5.3%) of the product as a solid.

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 twice by column chromatography on silica gel
6. additionFractions containing the product
7. customthe solvents evaporated