反应详情

温度

50 °C

100 mg of 2-[1-(4-ethoxy-2,6-difluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]-pyrazol-3-yl]-4-(pyridin-4-ylamino)pyrimidin-5-ol 2-2-1 (0.215 mmol, 1.00 eq.) were dissolved in 8 mL of dry DMF and 149 mg potassium carbonate (1.08 mmol, 5.00 eq.) and 47 mg 2-chloro-N,N-dimethylethanamine (0.323 mmol, 1.50 eq.) were added. The reaction mixture was stirred over night at 50° C. The reaction mixture was partitioned between aqueous half saturated sodium chloride solution and DCM/isopropanol (4:1). The separated aqueous layer was extracted with DCM/isopropanol (4:1). The combined organic layers were dried over magnesium sulfate and concentrated in vacuo. The purification of the residue by flash chromatography provided 51 mg (0.09 mmol, 42%) of analytically pure target compound.

1. customThe reaction mixture was partitioned between aqueous half saturated sodium chloride solution and DCM/isopropanol (4:1)
2. extractionThe separated aqueous layer was extracted with DCM/isopropanol (4:1)
3. dry with materialThe combined organic layers were dried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe purification of the residue by flash chromatography
6. customprovided 51 mg (0.09 mmol, 42%) of analytically pure target compound