反应详情

温度

100 °C

A mixture of 3-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene -2-carboxamide (100 mg, 0.45 mmol), 1-benzylpiperidin-4-one (0.093 mL, 0.50 mmol), CSA (125 mg, 0.54 mmol), MgSO4 (108 mg, 0.90 mmol) and DMA (1 mL) was stirred at 100° C. for 3 h. The mixture was poured into saturated aqueous NaHCO3. The organic materials were extracted with EtOAc. The combined extracts were washed with water and brine, and then dried over Na2SO4. After removal of the solvent at reduced pressure, the residue was purified by column chromatography (Purif, NH, 90:10 hexane/EtOAc to EtOAc then to 90:10 EtOAc/MeOH), then crystallized from MeOH/EtOAc/hexane to give the title compound (45 mg, 25%) as a yellow solid:

1. extractionThe organic materials were extracted with EtOAc
2. washThe combined extracts were washed with water and brine
3. dry with materialdried over Na2SO4
4. customAfter removal of the solvent at reduced pressure
5. customthe residue was purified by column chromatography (Purif, NH, 90:10 hexane/EtOAc to EtOAc
6. customto 90:10 EtOAc/MeOH), then crystallized from MeOH/EtOAc/hexane