反应详情

Methyl 2-(4-t -butylaminosulfonylphenyl) azulene-1-carboxylate: To a solution of methyl 2-chloroazulene-1-carboxylate (0.50 g) in toluene (20.0 ml) was added 4-t-butylaminosulfonyl-phenylboronic acid (0.87 g), tetrakis(triphenylphosphine)palladium (0) (0.12 g), and 2M aqueous Na2CO3 (4.5 ml), and the reaction mixture was heated under reflux for 16 hr. The mixture was poured into ice-water, followed by extracted with EtOAc. The combined EtOAc extracts were washed with water and brine, dried over Na2SO4, and concentrated. The crude product was purified by SiO2 column chromatography (CHCl3 /EtOAc, 100:1) to give the title compound (1.13 g) as violet crystals; mp 169°-170° C.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 16 hr
3. extractionby extracted with EtOAc
4. washThe combined EtOAc extracts were washed with water and brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. customThe crude product was purified by SiO2 column chromatography (CHCl3 /EtOAc, 100:1)