反应详情

温度

78 °C

0.3 g of 2-tert-Butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclopropyl-pyrimidine (0.89 mmol) were dissolved in 10 ml dimethylformamide. After the addition of 0.163 g 4-Methyl-5-trifluoromethyl-4H-[1,2,4]triazole-3-thiol (0.89 mmol), 0.064 g lithium hydroxide (2.76 mmol) and 0.067 g sodium iodide (0.45 mmol), the reaction mixture was stirred at 78° C. for 3 h. After cooling, the solvent was evaporated and the residue was dissolved in 30 ml of ethyl acetate. After washing twice with water, the organic phase was dried over magnesium sulfate, filtered, and the solvent was evaporated. The residue was purified chromatography on silica gel with ethyl acetate. Fractions containing the product were combined and the solvent was evaporated. The hydrochloride was formed by addition of 4 N HCl in dioxan to yield 0.14 g of the title compound.

1. temperatureAfter cooling
2. customthe solvent was evaporated
3. dissolutionthe residue was dissolved in 30 ml of ethyl acetate
4. washAfter washing twice with water
5. dry with materialthe organic phase was dried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent was evaporated
8. customThe residue was purified chromatography on silica gel with ethyl acetate
9. additionFractions containing the product
10. customthe solvent was evaporated