関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Glyoxylic Acid | HCID 760 | — |
| 反応物 | 2-Acetylthiophene | HCID 6920 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | trans-3-(2-Thenoyl)acrylic Acid | HCID 5773483 | 52.5% |
反応手順
A two phase mixture of 18 grams glyoxylic acid (an 80% solution of glyoxylic acid in water) and 25.2 grams of 2-acetylthiophene is heated to 125° C. with stirring, and heating and stirring are maintained for about 5 hours. A clear solution forms at 115° C. and the water formed is removed by means of a Dean-Stark apparatus. On cooling the residue solidifies. It is dissolved in 100 cc ether and extracted with 150 cc of a 20% solution of Na2CO3. This aqueous solution is treated with activated charcoal, filtered and made strongly acid with 20% HCl. The solid is filtered and dissolved in about 1 L ether. The ether is dried over MgSO4 and removed to yield 19.1 g of the title compound, melting point 139°-142° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04254267 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-adda741acd6c4f4b845bc6def37e7cfe |
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| 出典メモ | uspto-grants-1981_03 |
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