反应详情

温度

80 °C

100 mg of the 4-(8-hydroxyimidazo[1,2-a]pyridin-3-yl)-2-(methylthio)pyrimidine-5-carbonitrile [158-1] was dissolved in 3 mL of N,N-dimethylformamide, 146 mg of potassium carbonate and 216 mg of fluoromethyl 4-methylbenzenesulfonate (synthesized according to a method disclosed in page 555 to 566 in J. Labelled Compd. Radio pharm. 2003, 46) were added, and stirred at 80° C. for 5 hours. After cooling the reaction mixture back to room temperature, a saturated aqueous solution of sodium hydrogen carbonate was added, and was extracted with a mixture solvent of chloroform and methanol (chloroform:methanol=9:1). The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The insolubles were filtered, and the filtrate was concentrated under reduced pressure. The obtained residue was dissolved in a small amount of a mixture solvent of chloroform and methanol (chloroform:methanol=9:1), and solidified by adding diethyl ether, to obtain 44.1 mg of 4-[8-(fluoromethoxy)imidazo[1,2-a]pyridin-3-yl]-2-(methylthio)pyrimidine-5-carbonitrile [160-1] as a brown solid.

1. addition2003, 46) were added
2. temperatureAfter cooling the reaction mixture back to room temperature
3. extractionwas extracted with a mixture solvent of chloroform and methanol (chloroform:methanol=9:1)
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationThe insolubles were filtered
7. concentrationthe filtrate was concentrated under reduced pressure
8. dissolutionThe obtained residue was dissolved in a small amount of a mixture solvent of chloroform and methanol (chloroform:methanol=9:1)
9. additionby adding diethyl ether