反应详情

To a solution of 1,1-dimethylethyl 7-[(4-amino-2-fluorophenyl)oxy]-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (E274, Step 2) (0.5 g, 1.34 mmol) and iodoform (1 g, 2.69 mmol) in tetrahydrofuran (10 ml) was added dropwise tert-butyl nitrite (0.32 ml, 2.69 mmol). The reaction was then heated at reflux for 1 hour, cooled and concentrated in vacuo and resulting residue was purified by column chromatography eluting with a mixture of ethyl acetate:pentane (1:10) to afford the title compound. MS (ES+) m/e 384 [M−COOtBu]+.

1. temperatureThe reaction was then heated
2. temperatureat reflux for 1 hour
3. temperaturecooled
4. concentrationconcentrated in vacuo
5. customresulting residue
6. customwas purified by column chromatography
7. washeluting with a mixture of ethyl acetate:pentane (1:10)