反应详情

温度

60 °C

A mixture of 6-amino-5-chloro-2-oxo-N-(4-piperidinylmethyl)-1,2-dihydro-3-pyridinecarboxamide dihydrochloride (step 2, 100 mg, 0.28 mmol), iodoethane (49 mg, 0.31 mmol) and potassium carbonate (172 mg, 1.25 mmol) in N,N-dimethylformamide (6 ml) was stirred at 60° C. for 15 h. After cooling to room temperature, the solvent was removed in vacuo. The residue was suspended in tetrahydrofuran (50 ml), and the solution was filtered through a pad of Celite. The filtrate was concentrated in vacuo, and the obtained residue was chromatographed on a column of aminopropyl silica gel eluting with methanol/dichloromethane (1:2.5) to give 43 mg (49%) of the title compound as a white solid.

1. temperatureAfter cooling to room temperature
2. customthe solvent was removed in vacuo
3. filtrationthe solution was filtered through a pad of Celite
4. concentrationThe filtrate was concentrated in vacuo
5. customthe obtained residue was chromatographed on a column of aminopropyl silica gel eluting with methanol/dichloromethane (1:2.5)