反应详情

To a solution of methyl 2-[N-(2-oxopropyl)thiophene-3-yl-acetylamino]isobutyrate (7.6 g) in absolute ethanol (50 mL) was added 95% sodium methoxide (1.6 g), and the mixture was heated at reflux for 30 minutes. To the solution were added water (3.5 mL) and 85% potassium hydroxide (0.88 g), and the mixture was heated at reflux for 1 hour. After distilling off the solvent, the residue was poured into ice-water and washed with diethyl ether. It was adjusted to pH 2-3 with concentrated hydrochloric acid and the precipitated crystals were filtered, washed with water and dried to give 4.47 g of 2-[4-methyl-2-oxo-3-(thiophen-3-yl)-3-pyrrolin-1-yl]isobutyric acid.

1. temperaturethe mixture was heated
2. temperatureat reflux for 30 minutes
3. temperaturethe mixture was heated
4. temperatureat reflux for 1 hour
5. distillationAfter distilling off the solvent
6. additionthe residue was poured into ice-water
7. washwashed with diethyl ether
8. filtrationthe precipitated crystals were filtered
9. washwashed with water
10. customdried