反应详情

温度

50 °C

200 mg of 2-[1-(2-fluorobenzyl)-1H-indazol-3-yl]-4-(pyridin-4-ylamino)pyrimidin-5-ol (3-3, 0.49 mmol, 1 eq.), 94.6 mg of 2,2-dimethyl-4(R)-4-bromomethyl-1,3-dioxalane (0.49 mmol, 1 eq.) and 134 mg of potassium carbonate (0.97 mmol, 2 eq.) were suspended in 3.7 ml of dry DMF. The reaction mixture was stirred at 50° C. oil bath temperature for 18 hours. 201 mg of potassium carbonate (1.46 mmol, 3 eq.) were added and the mixture was stirred at 90° C. oil bath temperature for further 24 hours. Then the mixture was partitioned between half saturated aq. ammonium chloride solution and dichloromethane/isopropanol 4:1. The phases were separated and the aqueous layer was extracted twice with dichloromethane/isopropanol 4:1. The combined organic layers were washed with brine, dried over a silicone filter and concentrated in vacuo. The residue was purified by flash chromatography to yield 126 mg (0.27 mmol, 44%) of the analytically pure target compound.

1. stirringthe mixture was stirred at 90° C. oil bath temperature for further 24 hours
2. customThen the mixture was partitioned between half saturated aq. ammonium chloride solution and dichloromethane/isopropanol 4:1
3. customThe phases were separated
4. extractionthe aqueous layer was extracted twice with dichloromethane/isopropanol 4:1
5. washThe combined organic layers were washed with brine
6. dry with materialdried over a silicone
7. filtrationfilter
8. concentrationconcentrated in vacuo
9. customThe residue was purified by flash chromatography
10. customto yield 126 mg (0.27 mmol, 44%) of the analytically pure target compound