反应详情

温度

70 °C

0.2 g of 2-mercapto-pyridine (1.8 mmol) were dissolved in 15 ml of dimethylformamide. After addition of 0.04 g of lithium hydroxide (1.8 mmol) and 0.13 g of sodium iodide (0.9 mmol), the reaction mixture was stirred at 70° C. and 0.63 g of 2-tert-butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclobutyl-pyrimidine (0.9 mmol) were added in portions. The mixture was stirred at 80° C. for 5 h, and, after evaporation of dimethylformamide, the residue was partitioned between 20 ml of ethyl acetate and 15 ml of saturated aqueous sodium chloride solution and 15 ml of water. The aqueous phase was re-extracted twice with ethyl acetate. The combined organic layers were dried over magnesium sulfate, filtered, and concentrated to dryness. The crude product was purified by chromatography on silica gel using dichloromethane, dichloromethane-ethyl acetate (7:3-1:1). Fractions containing the product were combined. After evaporation of the solvent, the residue was re-dissolved in 20 ml of ethyl acetate and a 1 N solution of hydrochloric acid in diethyl ether was added. The precipitated hydrochloride salt was collected by filtration and dried to give 0.47 g of the title compound.

1. stirringThe mixture was stirred at 80° C. for 5 h
2. customafter evaporation of dimethylformamide
3. customthe residue was partitioned between 20 ml of ethyl acetate and 15 ml of saturated aqueous sodium chloride solution and 15 ml of water
4. extractionThe aqueous phase was re-extracted twice with ethyl acetate
5. dry with materialThe combined organic layers were dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated to dryness
8. customThe crude product was purified by chromatography on silica gel
9. additionFractions containing the product
10. customAfter evaporation of the solvent
11. dissolutionthe residue was re-dissolved in 20 ml of ethyl acetate
12. additiona 1 N solution of hydrochloric acid in diethyl ether was added
13. filtrationThe precipitated hydrochloride salt was collected by filtration
14. customdried