関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methyl 5-methyl-3,4-dihydroxy-2-furoate | HCID 54688627 | — |
| 反応物 | Ethyl 5-methyl-3,4-dihydroxy-2-furoate | HCID 54719681 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Furaneol | HCID 19309 | 76.6% |
反応手順
A solution of 32 g of sodium hydroxide and 33 g of a mixture containing 37.1% of methyl 5-methyl-3,4-dihydroxy-2-furoate and 52.1% of ethyl 5-methyl-3,4-dihydroxy-2-furoate in 320 ml of water was allowed to stand at room temperature for 20 hours. To the resulting mixture is added at 0° C. in one hour 25.2 g of dimethyl sulphate followed by an additional stirring period of three hours at 0° C. The pH of the solution was adjusted to 6.5 by the addition of concentrated hydrochloric acid solution. Extraction with methyl t-butyl ether yielded 18.1 g of 2,5-dimethyl-4-hydroxy-3[2H] furanone of 88.8% purity (molar yield 76.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05412121 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-e60933f0dafd4979a04714237e90ef77 |
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| 出典メモ | uspto-grants-1995_05 |
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