反应详情

温度

80 °C

3-[(4-Fluorophenyl)amino]-1H-pyrazole-4-carboxamide (Intermediate 31-7) (100 mg, 0.45 mmol) was added to a mixture of 2-(1,1-dioxidodihydro-2H-thiopyran-4(3H)-ylidene)acetonitrile (160 mg, 0.91 mmol) in MeCN (1.51 mL). DBU (0.068 mL, 0.45 mmol) was then added, the reaction vessel was capped and the reaction mixture was heated to 80° C. for 4 hours. The reaction mixture was cooled to ambient temperature, and purified by reverse phase preparative HPLC (using a gradient elution of MeCN/water, with 0.1% v/v TFA modifier). Desired fractions were combined, basified with saturated aqueous NaHCO3, and extracted with EtOAc. The organic layer was dried over anhydrous NaSO4, filtered, and concentrated in vacuo to afford the title compound, Example #7.

1. customthe reaction vessel was capped
2. temperatureThe reaction mixture was cooled to ambient temperature
3. custompurified by reverse phase preparative HPLC (
4. washa gradient elution of MeCN/water
5. extractionextracted with EtOAc
6. dry with materialThe organic layer was dried over anhydrous NaSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo