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Isopropanol → 5-Ethoxycarbonyl-3-isopropoxycarbonyl-1,4-dihydro-2,6-dimethyl-4-(3-ethynylphenyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Isopropyl acetoacetate | HCID 68329 | — |
| 反応物 | 2-Butenoic acid, 3-amino-, ethyl ester, (2Z)- | HCID 643756 | — |
| 反応物 | 3-Ethynylbenzaldehyde | HCID 2771644 | — |
| 触媒 | Piperidine | HCID 8082 | — |
| 生成物 | 5-Ethoxycarbonyl-3-isopropoxycarbonyl-1,4-dihydro-2,6-dimethyl-4-(3-ethynylphenyl)pyridine | HCID 19813405 | 58.6% |
反応手順
To a mixture of 0.65 g (0.005 mol) of 3ethynylbenzaldehyde, 1.08 g (0.0075 mol) of isopropyl acetoacetate and 25 ml of isopropyl alcohol were added 2 to 3 drops of piperidine. After heating the mixture under reflux for 24 hours, 0.65 g (0.005 mol) of ethyl 3-aminocrotonate was added thereto, further the admixture was heated under reflux for 24 hours. After completing the reaction, the reaction mixture was concentrated. The obtained precipitate was purified by subjecting to silica gel column chromatography [eluent: n-hexane to n-hexane: ethyl acetate (7 : 3)] to give 1.1 g of the desired compound (yield: 58.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05158963 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-d00579241cd841498e28cdd9874272dc |
| 出典メモ | uspto-grants-1992_10 |