反应详情

N-(1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-ylmethyl)-2-(2-oxo-2,3-dihydrobenzoimidazol-1-yl)-N-(2-pyridin-3-ylethyl)acetamide hydrochloride (0.26 g), cesium carbonate (0.43 g), and methyl iodide (0.04 ml) were added to DMF (5 ml), and the mixture was stirred at room temperature for 1 days. Water was added to the reaction mixture, and stirred for 1 hour, followed by extraction with ethyl acetate. The organic layer was condensed under reduced pressure, and the residue was purified by silica gel column chromatography (ethylacetate:methanol=85:15). The purified product was condensed under reduced pressure. A 1N-hydrogen chloride in ethanol solution (0.44 ml) was added to a 2-propanol solution (5 ml) of the residue, and the liquid was stirred at room temperature, and concentrated under reduced pressure. Ethanol and ether were added to the residue. The precipitated insoluble matter was separated, washed with ether, and dried to give the title compound (0.20 g) as a white powder.

1. stirringstirred for 1 hour
2. extractionfollowed by extraction with ethyl acetate
3. customcondensed under reduced pressure
4. customthe residue was purified by silica gel column chromatography (ethylacetate:methanol=85:15)
5. customcondensed under reduced pressure
6. stirringthe liquid was stirred at room temperature
7. concentrationconcentrated under reduced pressure
8. additionEthanol and ether were added to the residue
9. customThe precipitated insoluble matter was separated
10. washwashed with ether
11. customdried