反应详情

To 50 mL roundbottom flask containing trimethylsulfoxonium iodide (3.57 mmol, 785 mg) in DMSO (8 mL) was added potassium tert-butoxide (3.57 mmol, 401 mg). This suspension was allowed to stir at room temperature for 3 hours. After 3 hours, ethyl 2-(4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)pyrazolo[1,5-a]pyrimidin-5-yl)cyclohexylidene)acetate (1.78 mmol, 1.00 g) was added in 2 mL DMSO. The resulting solution was stirred at room temperature for 18 hours. After 18 hours, the reaction was diluted with saturated NaCl(aq) (30 mL). The pH was adjusted to ˜7 with saturated NH4Cl(aq) and extracted with DCM (50 mL) 4 times. The combined organics are dried over Na2SO4 and reduced in vacuo. The resulting residue was purified via flash chromatography to yield the title compound.

1. waitAfter 3 hours
2. stirringThe resulting solution was stirred at room temperature for 18 hours
3. waitAfter 18 hours
4. extractionextracted with DCM (50 mL) 4 times
5. dry with materialThe combined organics are dried over Na2SO4
6. customThe resulting residue was purified via flash chromatography