反应详情

Ethyl{ethoxycarbonyl[2-(5-methylfuran-2-yl)ethyl]-amino}acetate (0.65 g) prepared in the step 4 was dissolved in 5 mL of ethanol, 0.30 g of potassium hydroxide was added thereto and the mixture was heated to reflux for 3 hours. The solvent of the reaction solution was evaporated in vacuo and the residue was dissolved in ethyl acetate. The resulting solution was slowly neutralized with 1N aqueous solution of hydrochloric acid (ca. 80 mL) with stirring to adjust to pH 3. The organic layer was separated, washed with water and a saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom in vacuo. The residue was purified by silica gel column chromatography to give 0.18 g of the objective compound as yellow liquid.

1. temperaturethe mixture was heated
2. temperatureto reflux for 3 hours
3. customThe solvent of the reaction solution was evaporated in vacuo
4. dissolutionthe residue was dissolved in ethyl acetate
5. customThe organic layer was separated
6. washwashed with water
7. dry with materiala saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate
8. customthe solvent was evaporated
9. customThe residue was purified by silica gel column chromatography