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1,4-Dibromobutane → Diethyl tetrahydropyridazine-1,2-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,4-Dibromobutane | HCID 8056 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,2-Hydrazinedicarboxylic acid, 1,2-diethyl ester | HCID 77758 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Diethyl tetrahydropyridazine-1,2-dicarboxylate | HCID 281963 | 69.4% |
反応手順
1,4-Dibromobutane (81.4 mL, 0.682 mol) is added over 1 hour to a mixture of 1,2-dicarbethoxyhydrazine (100 g, 0.568 mol) and potassium carbonate (158 g, 1.14 mol) in acetonitrile (600 mL). The resultant reaction mixture is refluxed for 6 hours, cooled to room temperature, and filtered. The filtrate is concentrated in vacuo to obtain a yellow liquid which is distilled under reduced pressure to give the title product as a colorless liquid (90.8 g, bp 115°-120° C. at 0.9 mm Hg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05612481 |
| 出典データセット | uspto-grants-1997_03 |
| ORD ID | ord-ea5a11af08184d7f88095f37700274e8 |
| 出典メモ | uspto-grants-1997_03 |