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Ethyl cyanoacetate → Ethyl 4,6-dimethyl-2-oxo-1,2-dihydropyridine-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl cyanoacetate | HCID 7764 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | (3Z)-4-Amino-3-penten-2-one | HCID 5355751 | — |
| 生成物 | Ethyl 4,6-dimethyl-2-oxo-1,2-dihydropyridine-3-carboxylate | HCID 247443 | 19.9% |
反応手順
A solution of (Z)-4-aminopent-3-en-2-one (20.0 g, 0.2 mol) in dry THF (20 mL) is added to a solution of ethyl cyanoacetate (22.6 g, 0.2 mol) and TEA (20.2 g, 0.2 mol) in dry THF (200 mL). The reaction mixture is heated at reflux for 56 hours and then concentrated. The residue is kept standing at RT for 5 hours and the precipitate is filtered and washed with EtOAc to afford the title compound (7.3 g, 19.9% yield). MS (m/z): 196.0 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08030302B2 |
| 出典データセット | uspto-grants-2011_10 |
| ORD ID | ord-6c697817bdac4623b08e648de7cc0b58 |
| 出典メモ | uspto-grants-2011_10 |