Ethanol → 2-Ethoxycarbonylacetyl-3-hydroxy-thiophene

Participants

Reaction Steps

4.8 g (0.0337 mol) of 2-acetyl-3-hydroxythiophene in 150 ml of diethyl carbonate are heated to 90°-100° C. 5 g of small sodium pieces are then added. Stirring is continued for 15 hours at 90°-100° C. To decompose remainders of sodium, a little ethanol is added. For working up, the mixture is extracted twice using 75 ml of water, the aqueous phase is then acidified with 10 ml of concentrated HCl, extracted 3 times with 50 ml portions of ether, dried, distilled in vacuo, and the fraction between 70° and 100° C. (0.6 mbar, educt) and between 113° and 118° C. (0.4 mbar product) is collected.

Provenance & Evidence