反应详情

温度

125 °C

A two phase mixture of 18 grams glyoxylic acid (an 80% solution of glyoxylic acid in water) and 25.2 grams of 2-acetylthiophene is heated to 125° C. with stirring, and heating and stirring are maintained for about 5 hours. A clear solution forms at 115° C. and the water formed is removed by means of a Dean-Stark apparatus. On cooling the residue solidifies. It is dissolved in 100 cc ether and extracted with 150 cc of a 20% solution of Na2CO3. This aqueous solution is treated with activated charcoal, filtered and made strongly acid with 20% HCl. The solid is filtered and dissolved in about 1 L ether. The ether is dried over MgSO4 and removed to yield 19.1 g of the title compound, melting point 139°-142° C.

1. temperatureheating
2. stirringstirring
3. temperatureare maintained for about 5 hours
4. customis removed by means of a Dean-Stark apparatus
5. temperatureOn cooling the residue solidifies
6. dissolutionIt is dissolved in 100 cc ether
7. extractionextracted with 150 cc of a 20% solution of Na2CO3
8. additionThis aqueous solution is treated with activated charcoal
9. filtrationfiltered
10. filtrationThe solid is filtered
11. dissolutiondissolved in about 1 L ether
12. dry with materialThe ether is dried over MgSO4
13. customremoved