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Diethyl 2-(ethoxymethylidene)-3-oxobutanedioate → Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate
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 | Acetoacetamide | HCID 80077 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate | HCID 13752508 | — |
反応手順
Sodium acetate (30 g, 0.37 mol) is added to a stirred mixture of diethyl(ethoxymethylene)oxalacetate (87 g, 0.36 mol) and acetoacetamide (36 g, 0.36 mol) in absolute ethanol (300 mL). After stirring the reaction mixture for 30 minutes, the ethanol is distilled off under reduced pressure, the residue acidified to pH 2 with dilute aqueous hydrochloric acid and the resulting solid filtered off. Crystallization from an ethanol-water mixture affords diethyl 5-acetyl-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate as crystals mp 200°-209° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04701208 |
| 出典データセット | uspto-grants-1987_10 |
| ORD ID | ord-11ec135ee81b486d86692e51990b1186 |
| 出典メモ | uspto-grants-1987_10 |