反应详情

A mixture of 3-cyclobutyl-7-iodo-8-[(phenylmethyl)oxy]-2,3,4,5-tetrahydro-1H-3-benzazepine (E226) (250 mg, 0.58 mmol), tetrakis(triphenylphosphine)palladium (0) (33 mg, 0.029 mmol), copper (I) iodide (11 mg, 0.058 mmol) and sodium cyanide (56 mg, 1.15 mmol) in tetrahydrofuran (5 ml) was heated at reflux for 16 hours. The mixture was cooled and diluted with ethyl acetate, filtered through celite, washed with water then brine and dried over sodium sulfate and concentrated in vacuo. The crude mixture was purified by reverse phase HPLC to afford the title compound; MS (ES+) m/e 333 [M+H]+.

1. temperaturewas heated
2. temperatureat reflux for 16 hours
3. temperatureThe mixture was cooled
4. filtrationfiltered through celite
5. washwashed with water
6. dry with materialbrine and dried over sodium sulfate
7. concentrationconcentrated in vacuo
8. customThe crude mixture was purified by reverse phase HPLC