Reacción #156236
ord-2596dfbb3adc47489b70a46d9f61cf27
Ecuación de reacción
Reactantes
Reactivos
Disolventes
Condiciones de reacción
Tratamiento posterior
- 1TemperaturaThe reaction mixture was cooled to room temperature
- 2Extracciónfollowed by extraction by ethyl acetate
- 3LavadoThe organic layer was washed with water
- 4Secadowith saturated saline, and dried with anhydrous magnesium sulfate
- 5OtroAfter condensation under reduced pressure
- 6Otrothe residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1)
- 7Otrocondensed under reduced pressure
- 8workup.STIRRINGwas stirred at room temperature
- 9Otrocondensed to dryness under reduced pressure
Procedimiento
Potassium carbonate (0.54 g), sodium iodide (0.21 g), and 2-phenyl piperidine (0.23 g) were added to a DMF solution (15 ml) of 7-(3-chloropropoxy)-1-ethyl-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.44 g). The mixture was stirred at 70° C. for 5 hours. The reaction mixture was cooled to room temperature. Water was added thereto, followed by extraction by ethyl acetate. The organic layer was washed with water and then with saturated saline, and dried with anhydrous magnesium sulfate. After condensation under reduced pressure, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1). The purified product was condensed under reduced pressure. A 4N-Hydrogen chloride ethyl acetate solution (0.2 ml) was added to an ethyl acetate solution (10 ml) of the residue, which was stirred at room temperature. The liquid was condensed to dryness under reduced pressure to give the title compound (0.18 g) as a white amorphous solid.