反应详情

温度

60 °C

To a suspension of NaH (60% in mineral oil, 58 mg) in 10 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (320 mg, 1.04 mmol). The mixture was heated to 60° C. resulting in a clear solution. 1-Chloro-3-phenylpropane (260 μL, 1.81 mmol) was added, and the reaction mixture was heated at 60° C. for 35 minutes, then poured onto ice water. The resulting gummy solid was dissolved in ethyl acetate, washed with water, and dried over magnesium sulfate. Filtration, followed by concentration in vacuo, gave an oil that was purified by flash chromatography, eluting with 1:3 hexane:ethyl acetate to provide 345 mg of crude product. Recrystallization from ethyl acetate and hexane followed by drying in vacuo provided 253 mg (57%) of 2-amino-6-(2,6-dichlorophenyl)-8-(3-phenylpropyl)-8H-pyrido[2,3-d]pyrimidin-7-one; mp 161°-163° C.

1. customresulting in a clear solution
2. temperaturethe reaction mixture was heated at 60° C. for 35 minutes
3. additionpoured onto ice water
4. washwashed with water
5. dry with materialdried over magnesium sulfate
6. filtrationFiltration
7. concentrationfollowed by concentration in vacuo
8. customgave an oil that
9. customwas purified by flash chromatography
10. washeluting with 1:3 hexane
11. customethyl acetate to provide 345 mg of crude product
12. customRecrystallization from ethyl acetate and hexane
13. customby drying in vacuo