反应详情

1,1-dimethylethyl 7-hydroxy-8-[(methylsulfonyl)amino]-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (0.55 g) and 1,2-dibromoethane (0.23 ml) in the presence of potassium carbonate (0.4 g) were heated in acetone/water (1/1, 8 ml) for 6 h at reflux. Volatiles were evaporated under reduced pressure, the residue was partitioned between aqueous NaHCO3 and DCM. The organic layer was collected and the aqueous phase extracted twice with DCM. The combined organic layers were concentrated and submitted to column chromatography to provide the title compound (0.75 mmol) as a white slightly hygroscopic solid. MS (m/z): 383 [MH]+.

1. temperatureat reflux
2. customVolatiles were evaporated under reduced pressure
3. customthe residue was partitioned between aqueous NaHCO3 and DCM
4. customThe organic layer was collected
5. extractionthe aqueous phase extracted twice with DCM
6. concentrationThe combined organic layers were concentrated