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Diethyl 2-(ethoxymethylidene)-3-oxobutanedioate → Diethyl 5-ethylpyridine-2,3-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl 2-(ethoxymethylidene)-3-oxobutanedioate | HCID 40590 | — |
| 反応物 | 1-Morpholinobutene | HCID 580977 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Diethyl 5-ethylpyridine-2,3-dicarboxylate | HCID 10857926 | 57% |
反応手順
Diethyl ethoxymethyleneoxalacetate (3.17 g, 0.013 mol) is added to a solution of 1-morpholinobutene (1.84 g, 0.013 mol) dissolved in CH2Cl2 (40 mL) at 0°. The solution is concentrated in vacuo, and ammonium acetate (50 g), ammonium hydroxide (10 mL), tetrahydrofuran (20 mL) and 95% ethanol (20 mL) are added. The solution is heated to reflux for 30 minutes, then held at 3° for 72 hours. The reaction solution is then partitioned between water and ethyl acetate. The organic layer is dried over sodium sulfate and concentrated in vacuo to give the product (1.85 g, 0.0074 mol, 57%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05563113 |
| 出典データセット | uspto-grants-1996_10 |
| ORD ID | ord-d38d8bd747454887a4f19a9e5a72c093 |
| 出典メモ | uspto-grants-1996_10 |