反应详情

温度

80 °C

A mixture of 3-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene -2-carboxamide (66 mg, 0.30 mmol), 2-fluorocyclohexanone (0.10 mL, 0.90 mmol), CSA (7.0 mg, 0.030 mmol), MgSO4 (72 mg, 0.60 mmol) and DMA (1 mL) was stirred at 80° C. for 2 h. Then, saturated aqueous NaHCO3 and EtOAc were added to quench the reaction. The organic materials were extracted with EtOAc. The combined extracts were washed with water and brine, dried over Na2SO4. After removal of the solvent at reduced pressure, the residue was purified by column chromatography (Purif, silica gel 85:15 hexane/EtOAc to EtOAc), then crystallized from MeOH/EtOAc/hexane) to give the title compound (53 mg, 55%) as a pale yellow solid:

1. customto quench
2. customthe reaction
3. extractionThe organic materials were extracted with EtOAc
4. washThe combined extracts were washed with water and brine
5. dry with materialdried over Na2SO4
6. customAfter removal of the solvent at reduced pressure
7. customthe residue was purified by column chromatography (Purif, silica gel 85:15 hexane/EtOAc to EtOAc)
8. customcrystallized from MeOH/EtOAc/hexane)