反应详情

温度

60 °C

0.4 g of 2-mercapto-pyrimidine (3.57 mmol) were dissolved in 20 ml of dimethylformamide. After addition of 0.09 g of lithium hydroxide (3.57 mmol) and 0.27 g of sodium iodide (1.78 mmol), the reaction mixture was stirred at 60° C. and 1.25 g of 2-tert-butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclobutyl-pyrimidine (3.57 mmol) were added in portions. The mixture was stirred at 60° C. for 1 h. After cooling, the dimethylformamide was evaporated and the residue was partitioned between 30 ml of ethyl acetate and half-saturated sodium chloride solution (15 ml of saturated aqueous sodium chloride solution and 15 ml of water). The aqueous phase was reextracted twice with ethyl acetate. The combined organic layers were dried over magnesium sulfate, filtered, and concentrated to dryness. The crude product was redissolved in 30 ml of ethyl acetate. The hydrochloride was formed by addition of 4 N hydrochloric acid in dioxane to yield 1.8 g of the title compound as a crystallized hydrochloride salt.

1. stirringThe mixture was stirred at 60° C. for 1 h
2. temperatureAfter cooling
3. customthe dimethylformamide was evaporated
4. customthe residue was partitioned between 30 ml of ethyl acetate and half-saturated sodium chloride solution (15 ml of saturated aqueous sodium chloride solution and 15 ml of water)
5. dry with materialThe combined organic layers were dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated to dryness
8. dissolutionThe crude product was redissolved in 30 ml of ethyl acetate