反应详情

温度

120 °C

Methyl 2-(4-methylsulfonylphenyl)-3-phenylazulene-1-carboxylate(0.13 g) was treated with 100% phosphoric acid (5.0 ml). After stirring for 10 min at 120° C., the reaction 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 (benzenee/Et2O, 50: 1) to give the title compound (0.10 g) as violet crystals; mp 139°-140° C.

1. extractionby extracted with EtOAc
2. washThe combined EtOAc extracts were washed with water and brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. customThe crude product was purified by SiO2 column chromatography (benzenee/Et2O, 50: 1)