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Acetic Acid → Furaneol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Bismuth-oxygen | HCID 6327914 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Bismuth acetate | HCID 31132 | — |
| 溶媒 | Bismuth | HCID 5359367 | — |
| 生成物 | Furaneol | HCID 19309 | 79% |
反応手順
17.5 g of 2,5-dimethyl-3,4-dihydroxy-tetrahydrofuran-3-one of about 80% purity were heated, in a suspension of 40 g of bismuth oxide and 50 g of glacial acetic acid, for 25 minutes at 120° C. After the reaction mixture had cooled, it was diluted with 80 g of ethyl acetate, whereupon metallic bismuth and bismuth acetate precipitated. The filtrate was fractionated, giving, at 85°-101° C./0.3 mbar, 14.2 g of a distillate containing about 77% of (I). This corresponds to a yield of 79%. 2.5 g of this fraction were taken up in a mixture of 2.8 g of chloroform and 1.6 g of petroleum ether, from which, after cooling, pure (I) of solidification point 75°-76° C. crystallized.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04290960 |
| 出典データセット | uspto-grants-1981_09 |
| ORD ID | ord-85f6e485a94c4add8531a1afbca660c3 |
| 出典メモ | uspto-grants-1981_09 |