反应详情

In a pressure tube reactor, ((S)-5-(1-((4-(5-bromopyrimidin-2-yl)morpholine-2-yl)methyl)-1H-[1,2,3]triazolo[4,5-b]pyrazin-6-yl)-2-fluorobenzonitrile 100 mg (0.20 mmol) was added, and potassium carbonate 83 mg (0.60 mmol) was added. Pd(dppf)2Cl2 8 mg (0.01 mmol) was further added, followed by 1,4-dioxane 3 ml, tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolane-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate 74 mg (0.24 mmol), and H2O 0.5 ml. The mixture was stirred at room temperature for 10 minutes under nitrogen gas, and then stirred at 80° C. for 2 hours. When the reaction was completed, the organic layer was extracted with ethyl acetate and water, and the extra water was removed by sodium sulfate, followed by concentration under reduced pressure. Column chromatography using 50% ethylacetate/hexane gave (S)-tert-butyl 4-(2-(2-((6-(3-cyano-4-fluorophenyl)-1H-[1,2,3]triazolo[4,5-b]pyrazin-1-yl)methyl)morpholino)pyrimidin-5-yl)-5,6-dihydropyridine-1(2H)-carboxylate 104 mg (0.17 mmol) with a yield of 87%.

1. stirringstirred at 80° C. for 2 hours
2. extractionthe organic layer was extracted with ethyl acetate and water
3. customthe extra water was removed by sodium sulfate
4. concentrationfollowed by concentration under reduced pressure