反应详情

Methyl 3-bromo-2-(4-t-butylaminosulfonylphenyl) azulene-1-carboxylate: To a solution of 2-(4-t - butylaminosulfonylphenyl) -1-phenylazulene (0.50 g) in CCl4 (20.0 ml) was added N-bromosuccinimide (0.25 g) and α,α'-azobis (isobutyronitrile) (0.01 g), and the reaction mixture was heated under reflux for 1 hr. The reaction mixture was filtered, and concentrated. The crude product was purified by SiO2 column chromatography (benzene/EtOAc, 20:1) to give the title compound (0.56 g) as violet crystals; mp 171°-172° C.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 1 hr
3. filtrationThe reaction mixture was filtered
4. concentrationconcentrated
5. customThe crude product was purified by SiO2 column chromatography (benzene/EtOAc, 20:1)