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Isobutyl acetoacetate → 4-(2,1,3-Benzoxadiazol-4-yl)-2,6-dimethyl-1,4-dihydro-3-methoxy carbonyl-pyridine-5-carboxylic acid isobutyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isobutyl acetoacetate | HCID 522677 | — |
| 反応物 | Methyl 3-aminocrotonate | HCID 643918 | — |
| 反応物 | 2,1,3-Benzoxadiazole-4-carbaldehyde | HCID 10290873 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(2,1,3-Benzoxadiazol-4-yl)-2,6-dimethyl-1,4-dihydro-3-methoxy carbonyl-pyridine-5-carboxylic acid isobutyl ester | HCID 13231102 | — |
反応手順
3 g of 2,1,3-benzoxadiazole-4-aldehyde, 3.2 g of acetoacetic acid isobutyl ester, 2.3 g β-aminocrotonic acid methyl ester and 10 ml of ethanol are stirred under reflux for 3 hours. The mixture is subsequently evaporated and the residue is chromatographed on silica gel with chloroform/acetic acid ethyl ester (8:1) to yield the title compound. The product is recrystallised from diisopropyl ether and methylcyclohexane, m.p. 148°-158°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04567271 |
| 出典データセット | uspto-grants-1986_01 |
| ORD ID | ord-19f56ac2a5814730b77eb37b2ee022b9 |
| 出典メモ | uspto-grants-1986_01 |