反应详情

5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-ol (11.7 mmol) is charged to 250 mL roundbottom flask. To this flask is added 4 mL N,N-dimethylaniline, followed by 40 mL POCl3. This suspension was sonicated to break up the starting material and stirred at room temperature for 18 hours. After 18 hours, a solution formed. The solution was reduced in vacuo and cooled to 0° C. in ice bath. The reaction is then quenched with sat. NaHCO3(aq) and extracted with DCM (×3). The combined organics are dried with Na2SO4 and the solvent was removed in vacuo. The resulting oil was purified via silica gel column on 20% to 100% ethyl acetate in hexanes gradient to yield 7-chloro-5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidine (2.65 grams, 77% across 2 steps) as white solid.

1. customThis suspension was sonicated
2. waitAfter 18 hours
3. customa solution formed
4. temperaturecooled to 0° C. in ice bath
5. customThe reaction is then quenched with sat. NaHCO3(aq)
6. extractionextracted with DCM (×3)
7. dry with materialThe combined organics are dried with Na2SO4
8. customthe solvent was removed in vacuo
9. customThe resulting oil was purified via silica gel column on 20% to 100% ethyl acetate in hexanes gradient