反应详情

The mixture of methyl 3-aminobenzoate (110.0 g) and 2,5-dimethoxytetrahydrofuran (141.4 ml) in acetic acid (330 ml) was heated under reflux for 50 minutes under stirring and the solvent was removed by concentration in vacuo. To the residue was added a mixture of ethyl acetate and water, and adjusted to pH 8 with potassium carbonate. The separated organic layer was washed with water and dried over magnesium sulfate. Evaporation of a solvent gave a residue, which was purified by column chromatography on silica gel eluting with chloroform. The eluted fractions containing the desired product were collected and evaporated in vacuo to give methyl 3-(pyrrol-1-yl)benzoate (112.84 g) as an oil.

1. temperaturewas heated
2. temperatureunder reflux for 50 minutes
3. customthe solvent was removed by concentration in vacuo
4. additionTo the residue was added
5. additiona mixture of ethyl acetate and water
6. washThe separated organic layer was washed with water
7. dry with materialdried over magnesium sulfate
8. customEvaporation of a solvent
9. customgave a residue, which
10. customwas purified by column chromatography on silica gel eluting with chloroform
11. additionThe eluted fractions containing the desired product
12. customwere collected
13. customevaporated in vacuo