関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 1,1-Dichloroethane | HCID 6365 | — |
| 反応物 | Methyl acetoacetate | HCID 7757 | — |
| 反応物 | 2-(Acetyloxy)propanal | HCID 90728 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Furancarboxylic acid, 2,5-dimethyl-, methyl ester | HCID 80248 | — |
反応手順
12.2 parts by weight of anhydrous iron-III chloride followed by 44.9 parts by weight of 85.5 percent strength by weight α-acetoxypropionaldehyde are added to a solution of 34.8 parts by weight of methyl acetoacetate in 36 parts by weight of methanol, during which addition the mixture rises to the boil. The mixture is then refluxed for a further 1-6 hours and, when it has cooled, is mixed with 80 parts by weight of water and 37.5 parts by weight of dichloroethane; the water phase is separated off and is extracted twice, each time with 25 parts by weight of dichloroethane. The dichloroethane is distilled off under atmospheric pressure and the product is then distilled under reduced pressure. 39 parts by weight of 2,5-dimethylfuran-3-carboxylic acid methyl ester of boiling point 92° C./26 mbar are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04207243 |
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| 出典データセット | uspto-grants-1980_06 |
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| ORD ID | ord-070831e44dd6489fbf0c38adfbe88d25 |
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| 出典メモ | uspto-grants-1980_06 |
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