関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Ethyl orthoformate | HCID 31214 | — |
| 生成物 | Butanoic acid, 2-(ethoxymethylene)-3-oxo-, ethyl ester | HCID 97734 | 70% |
反応手順
A mixture of ethyl acetoacetate (100 g, 0.77 mol), triethyl orthoformate (130 g, 0.92 mol), and acetic anhydride (150 g, 1.5 mol) was heated at 135° C. for 6-18 h in a round bottomed flask that was equipped with a distillation apparatus to collect the ethanol generated during the reaction. The reaction was cooled, concentrated and the residue was distilled under high vacuum to obtain the desired product (100 g, 70%) as a pale yellow oil: ESI MS m/z 187 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09345709B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-8570c88f10834a9a95744fb4189550c1 |
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| 出典メモ | uspto-grants-2016_05 |
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