참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Glyoxylic Acid | HCID 760 | — |
| 반응물 | 2-Acetylfuran | HCID 14505 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 4-(2-Furanyl)-4-oxo-2-butenoic acid | HCID 54249028 | 21.7% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04254267 |
|---|
| 출처 데이터셋 | uspto-grants-1981_03 |
|---|
| ORD ID | ord-5913ae38c5a145c4b87f0c357caf8b6a |
|---|
| 출처 메모 | uspto-grants-1981_03 |
|---|