反应详情

To a solution of methyl 2 -(4-methylsulfonylphenyl)-3-phenylazulene-1-carboxylate (0.26 g) in MeOH (10.0 ml) was added 10% aqueous NaOH (2.0 ml), and the reaction mixture was heated under reflux for 6 hr. After removal of solvent, the aqueous layer was washed with Et2O. The solution was adjusted to pH 2.0 with 10% aqueous HCl, and 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 (EtOAc/MeOH, 30: 1) to give the title compound (0.20 g) as violet crystals; mp 168°-169° C.

1. temperaturethe reaction mixture was heated
2. temperatureunder reflux for 6 hr
3. customAfter removal of solvent
4. washthe aqueous layer was washed with Et2O
5. extractionextracted with EtOAc
6. washThe combined EtOAc extracts were washed with water and brine
7. dry with materialdried over Na2SO4
8. concentrationconcentrated
9. customThe crude product was purified by SiO2 column chromatography (EtOAc/MeOH, 30: 1)