反应详情

A stirred solution of 2-amino-1-(2-phenyl-4H-[1,3]dioxino[5,4-b]pyridin-6-yl)ethanol (100 mg) (EP220054A2), diisopropylethylamine (0.08 ml) and 3-{4-[(6-bromohexyl)oxy]butyl}benzenesulfonamide (120 mg) in N,N-dimethylformamide (2 ml) under nitrogen was heated to 50° for 18 h. The mixture was cooled to 20° and the solvent evaporated in vacuo. The residue was dissolved in acetic acid (4 ml) and water (2 ml) and was heated to 70° for 18 h. The mixture was cooled to 20°, the solvent evaporated in vacuo and the residue purified by mass-directed autopreparative HPLC to give the title compound (22 mg). LCMS RT=2.23 min, ES+ve 496 (MH)+.

1. temperatureThe mixture was cooled to 20°
2. customthe solvent evaporated in vacuo
3. dissolutionThe residue was dissolved in acetic acid (4 ml)
4. temperaturewater (2 ml) and was heated to 70° for 18 h
5. temperatureThe mixture was cooled to 20°
6. customthe solvent evaporated in vacuo
7. customthe residue purified by mass-directed autopreparative HPLC