反应详情

A mixture of 14.8 g of glyoxylic acid (in 18.5 cc of water) and 22 g of 2-acetylfuran is heated at 125°-135° C. for about 5 hours; the water is removed as it forms via a Dean Stark tube. The mass cyrstallizes over about a 16 hour period and is dissolved in 600 cc of ethyl acetate and extracted into 600 cc of 10% sodium carbonate. The aqueous solution is treated with activated charcoal and a filter aid, and then filtered. It is made strongly acid with 20% HCl and the solid which precipitates is extracted with ethyl acetate. The ethyl acetate is dried over MgSO4 and removed to yield a solid residue which is dissolved in 100 cc hot acetonitrile and allowed to cool for about 16 hours. The solid is filtered to yield 7.2 g of the title compound, melting point 153°-155° C.

1. temperatureis heated at 125°-135° C. for about 5 hours
2. customthe water is removed as it
3. customcyrstallizes over about a 16 hour period
4. dissolutionis dissolved in 600 cc of ethyl acetate
5. extractionextracted into 600 cc of 10% sodium carbonate
6. additionThe aqueous solution is treated with activated charcoal
7. filtrationa filter aid, and then filtered
8. customthe solid which precipitates
9. extractionis extracted with ethyl acetate
10. dry with materialThe ethyl acetate is dried over MgSO4
11. customremoved
12. customto yield a solid residue which
13. temperatureto cool for about 16 hours
14. filtrationThe solid is filtered