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Ethanol → 5-Isopropoxycarbonyl-1,4-dihydro-2,6-dimethyl-3-methoxyethoxycarbonyl-4-(3-ethynylphenyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 2-Methoxyethyl acetoacetate | HCID 89734 | — |
| 反応物 | 3-Ethynylbenzaldehyde | HCID 2771644 | — |
| 反応物 | 2-Butenoic acid, 3-amino-, 1-methylethyl ester | HCID 11137274 | — |
| 生成物 | 5-Isopropoxycarbonyl-1,4-dihydro-2,6-dimethyl-3-methoxyethoxycarbonyl-4-(3-ethynylphenyl)pyridine | HCID 19813419 | 53% |
反応手順
In 30 ml of dry ethyl alcohol was dissolved 1.3 g (10 mmol) of 3-ethynylbenzaldehyde, and 1.43 g (10 mmol) of isopropyl 3-aminocrotonate and 1.6 g (10 mmol) of methoxyethyl acetoacetate were successively added thereto at room temperature. The admixture was reacted under reflux with heating for 12 hours. After completing the reaction, the reaction solution was distilled away under reduced pressure and purified by subjecting to silica gel column chromatography [eluent: n-hexane-chloroform (1 : 1) to chloroform]to give 2.1 g of the chloroform (1 : 1) to chloroform] to give 2.1 g of the desired compound (yield: 53%).
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-d5704b7d097b4eca9c81603ae798a68b |
| 出典メモ | uspto-grants-1992_10 |