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Cyanoacetamide → 5-Ethyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyanoacetamide | HCID 7898 | — |
| 反応物 | 2-Ethyl-3-oxobutanol | HCID 270299 | — |
| 反応物 | Piperidinium acetate | HCID 3014295 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Ethyl-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile | HCID 10241109 | — |
反応手順
Accordingly to the method described in J. Heterocyclic Chem., 24, 351 (1987), a mixture 2-ethyl-3-oxobutanol, sodium salt (37.5 g, 0.275 mol), cyanoacetamide (25.2 g, 0.30 mol), aqueous piperidinium acetate (22 mL) [prepared from glacial acetic acid (4.2 mL), water (10 mL) and piperidine (7.2 mL)] in water (775 ml) was refluxed for four hours. Glacial acetic acid (30 ml) was added cautiously (much foaming) as the product precipitated. Upon cooling to room temperature, the product was collected by filtration, washed with cold water and air dried to yield 22.3 g (50%), m.p. 237°-240° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05387512 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-3a7b3ceddd7744df9e57264e8f93a1de |
| 出典メモ | uspto-grants-1995_02 |