反应详情

温度

150 °C

461 mg of 2-[1-(4-ethoxy-2,6-difluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]-pyrazol-3-yl]-5-methoxy-N-(pyridin-4-yl)pyrimidin-4-amine 2-1-1 (0.964 mmol, 1.00 eq.) were dissolved in 42 mL of dry 1-methylpyrrolidin-2-one. 51 mg of potassium carbonate (0.366 mmol, 0.38 eq.) and 150 μL benzenethiol (1.45 mmol, 1.5 eq.) were added. The mixture was stirred for 1 h at 150° C. bath temperature. The reaction mixture was partitioned between aqueous half saturated ammonium chloride solution and DCM/isopropanol (4:1). The separated aqueous layer was extracted twice 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 349 mg (0.75 mmol, 78%) of analytically pure target compound.

1. customThe reaction mixture was partitioned between aqueous half saturated ammonium chloride solution and DCM/isopropanol (4:1)
2. extractionThe separated aqueous layer was extracted twice 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 349 mg (0.75 mmol, 78%) of analytically pure target compound