反应详情

温度

70 °C

0.21 g of 4-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 2 h, and after evaporation of dimethylformamide, 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 reextracted 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 with ethyl acetate and ethyl acetate-methanol (9:1). Fractions containing the product were combined. After evaporation of the solvent, the residue was re-dissolved in 15 ml of ethyl acetate and 1 N solution of hydrochloric acid in diethyl ether was added. The precipitated hydrochloride salt was collected by filtration and dried to give 0.54 g of the title product.

1. stirringThe mixture was stirred at 80° C. for 2 h
2. customafter evaporation of dimethylformamide
3. custompartitioned between 20 ml of ethyl acetate and 15 ml of saturated aqueous sodium chloride solution and 15 ml of water
4. dry with materialThe combined organic layers were dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated to dryness
7. customThe crude product was purified by chromatography on silica gel with ethyl acetate and ethyl acetate-methanol (9:1)
8. additionFractions containing the product
9. customAfter evaporation of the solvent
10. dissolutionthe residue was re-dissolved in 15 ml of ethyl acetate
11. addition1 N solution of hydrochloric acid in diethyl ether was added
12. filtrationThe precipitated hydrochloride salt was collected by filtration
13. customdried