反应详情

温度

80 °C

A mixture of 3-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene -2-carboxamide (111 mg, 0.50 mmol), 2-indanone (330 mg, 2.50 mmol), MgSO4 (120 mg, 1.00 mmol), CSA (11.6 mg, 0.050 mmol) and DMA (3 mL) was stirred at 80° C. for 1 h. The mixture was poured into saturated aqueous NaHCO3 and 2:1 EtOAc/THF. The organic layer was collected, dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (Purif, silica gel, hexane to EtOAc, then to 90:10 EtOAc/MeOH), then triturated with EtOAc, and the precipitate was collected by filtration to afford the title compound (21 mg, 12%) as a beige solid:

1. customThe organic layer was collected
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by column chromatography (Purif, silica gel, hexane to EtOAc
6. customto 90:10 EtOAc/MeOH), then triturated with EtOAc
7. filtrationthe precipitate was collected by filtration