反应详情

温度

60 °C

(Dimethylamino)sulfur trifluoride (0.010 ml, 0.18 mmol) was added to a stirred solution of 9-(1-hydroxy-2-morpholinoethyl)-6-(4-methoxybenzyl)pyrido[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5(6H)-one (49 mg, 0.090 mmol) in acetonitrile (1 ml). After 4 hours, additional (dimethylamino)sulfur trifluoride (0.035 ml, 0.36 mmol) was added and the mixture was stirred at 60° C. for 20 hours, cooled to room temperature, diluted with aqueous sodium bicarbonate (3 mL) and extracted with DCM (2×3 mL). The combined extracts were concentrated under a stream of nitrogen and the residue was taken up in methanol, filtered and purified by preparative HPLC. The resulting material retained some impurities so it was diluted with aqueous sodium bicarbonate (3 mL) and extracted with DCM (2×3 mL). The combined extracts were concentrated under a stream of nitrogen and the residue was purified by flash chromatography (elution with 0-40% IPA in ethyl acetate) to afford 9 mg (21%) of 269 as a white powder.

1. temperaturecooled to room temperature
2. extractionextracted with DCM (2×3 mL)
3. concentrationThe combined extracts were concentrated under a stream of nitrogen
4. filtrationfiltered
5. custompurified by preparative HPLC
6. additionwas diluted with aqueous sodium bicarbonate (3 mL)
7. extractionextracted with DCM (2×3 mL)
8. concentrationThe combined extracts were concentrated under a stream of nitrogen
9. customthe residue was purified by flash chromatography (elution with 0-40% IPA in ethyl acetate)