反应详情

温度

70 °C

0.7 g of 2-tert-Butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclopropyl-pyrimidine (1.45 mmol) and 0.55 g of 4-methyl-4H-[1,2,4]triazole-3-thiol (2.08 mmol) were dissolved in 10 ml of dimethylformamide. After addition of 0.104 g of lithium hydroxide (4.36 mmol) and 0.109 g of sodium iodide (0.73 mmol), the reaction mixture was stirred at 70° C. for 3 h. After cooling, the solvent was evaporated and the residue partitioned between dichloromethane and half-saturated sodium chloride solution. The organic layer was dried over magnesium sulfate, filtered, and the solvent was evaporated. The residue was purified via preparative HPLC on a C18-Symmetry column (Waters) with water/methanol (0.1% acetic acid). Fractions containing the product were combined and lyophilised to yield 0.075 g of the product.

1. temperatureAfter cooling
2. customthe solvent was evaporated
3. customthe residue partitioned between dichloromethane and half-saturated sodium chloride solution
4. dry with materialThe organic layer was dried over magnesium sulfate
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe residue was purified via preparative HPLC on a C18-Symmetry column (Waters) with water/methanol (0.1% acetic acid)
8. additionFractions containing the product