化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Dimethyl 2-methyl-3-hydroxy-6-vinylpyridine 4,5-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Dimethyl maleate | HCID 5271565 | — |
| 反応物 | 5-Ethoxy-4-methyl-2-vinyloxazole | HCID 20263981 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Dimethyl 2-methyl-3-hydroxy-6-vinylpyridine 4,5-dicarboxylate | HCID 20263984 | — |
反応手順
A mixture of0.2 mole of dimethyl maleate and 0.1 mole of 5-ethoxy-4-methyl-2-vinyloxazole are heated at 110°-115° C. for 4 hours. The reaction mixture is cooled and 20 ml. of a 25% solution of hydrogen chloride (dry) in absolute methanol added. Addition of ether to the cooled reaction mixture precipitates the hydrochloride salt of the product. The free base is obtained by dissolving the hydrochloride salt in a minimum volume of water, adding solid sodium bicarbonate to pH 6.5 to 7.0 and extracting with chloroform. The combined chloroform extracts are dried over sodium sulfate and concentrated in vacuo to give dimethyl 2-methyl-3-hydroxy-6-vinylpyridine 4,5-dicarboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04355034 |
| 出典データセット | uspto-grants-1982_10 |
| ORD ID | ord-08f277896c464e05a168dd5b5710a2ca |
| 出典メモ | uspto-grants-1982_10 |