反应详情

To a solution of 1-methoxycarbonylmethoxy-5-oxo-5,6,7,8-tetrahydronaphthalene (0.5 g) in dry dichloromethane (3 ml) was added bromine (0.14 ml) at 0° C. The mixture was warmed up to room temperature, stirred for 2 hours. The mixture was washed with an aqueous saturated sodium bicarbonate, dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel (30 ml) using a mixture of dichloromethane--n-hexane. The desired fractions were collected and evaporated in vacuo to give 1-methoxycarbonylmethoxy-5-oxo-6-bromo-5,6,7,8-tetrahydronaphthalene (0.41 g). The crude crystal (50 mg) was recrystallized from ethyl acetate--n-hexane to give 31 mg as a white crystal.

1. washThe mixture was washed with an aqueous saturated sodium bicarbonate
2. dry with materialdried over magnesium sulfate
3. customevaporated in vacuo
4. customThe residue was chromatographed on silica gel (30 ml)
5. additiona mixture of dichloromethane
6. customThe desired fractions were collected
7. customevaporated in vacuo