反应详情

To a 100 mL round-bottom flask was charged ethyl 4-((7-hydroxypyrazolo[1,5-a]pyrimidin-5-yl)methyl)cyclohexanecarboxylate (Int-4f, 2.48 g, 8.19 mmol), N,N-dimethylaniline (4 mL) and POCl3 (40 mL). The resulting solution was allowed to stir at room temperature for 18 hours. After 18 hours, the solvent was removed in vacuo. The residue was cooled to 0° C. in ice bath. The cooled residue was slowly quenched with saturated NaHCO3 (aq), and then extracted with DCM (x3). The combined organic extracts were dried over Na2SO4 and the residue purified via silica gel chromatography to yield the title compound as clear oil. Yield=2.29 g.

1. waitAfter 18 hours
2. customthe solvent was removed in vacuo
3. temperatureThe residue was cooled to 0° C. in ice bath
4. customThe cooled residue was slowly quenched with saturated NaHCO3 (aq)
5. extractionextracted with DCM (x3)
6. dry with materialThe combined organic extracts were dried over Na2SO4
7. customthe residue purified via silica gel chromatography