反应详情

Methanol (20 ml) was added dropwise to a mixture of dimethyl 5-iodoisophthalate (20.0 g) and sodium borohydride (2.4 g) in tetrahydrofuran (200 ml) for 15 minutes at 45-50° C., and the mixture was stirred for 1 hour at same temperature. The reaction mixture was added to a mixture of ethyl acetate and water, and the separated organic layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel with chloroform-methanol (19:1, V/V) as an eluent. The fractions containing the desired product were collected and evaporated in vacuo to give methyl 5-hydroxymethyl-3-iodobenzoate (15.11 g).

1. washthe separated organic layer was washed with brine
2. dry with materialdried over magnesium sulfate
3. customevaporated in vacuo
4. customThe residue was purified by column chromatography on silica gel with chloroform-methanol (19:1, V/V) as an eluent
5. additionThe fractions containing the desired product
6. customwere collected
7. customevaporated in vacuo