反应详情

温度

100 °C

A mixture of 3-amino-5-(5-methyl-1H-pyrazol-4-yl)thiophene -2-carboxamide (111 mg, 0.50 mmol), N-(4-fluorophenyl)-piperidin-4-one (290 mg, 1.50 mmol), MgSO4 (120 mg, 1.00 mmol), CSA (11.6 mg, 0.05 mmol) and DMA (4 mL) was stirred at 100° C. for 1 h. The mixture was poured into saturated aqueous NaHCO3 and extracted with 3:1 EtOAc/THF, and the extract was dried over MgSO4 and concentrated under reduced pressure. The residue was purified by column chromatography (Purif, silica gel, EtOAc to 80:20 EtOAc/MeOH). The obtained residue was triturated with EtOAc, and the precipitates were collected by filtration to afford the title compound (102 mg, 51%) as a light yellow solid:

1. extractionextracted with 3:1 EtOAc/THF
2. dry with materialthe extract was dried over MgSO4
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by column chromatography (Purif, silica gel, EtOAc to 80:20 EtOAc/MeOH)
5. customThe obtained residue was triturated with EtOAc
6. filtrationthe precipitates were collected by filtration