関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Nitrobenzaldehyde | HCID 7449 | — |
| 反応物 | 2-Butenoic acid, 3-amino-, ethyl ester, (2Z)- | HCID 643756 | — |
| 反応物 | 2-(4-Acetylaminobenzoyloxy)ethyl acetylacetate | HCID 20151269 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(4-Acetylaminobenzoyloxy)ethyl 2,6-dimethyl-5-ethoxycarbonyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylate | HCID 20151280 | 46% |
反応手順
20 g (0.07 moles) of 2-(4-acetylaminobenzoyloxy)ethyl acetylacetate, 8.41 (0.07 moles) of ethyl 3-aminocrotonate and 9.84 g (0.07 moles) of 3-nitrobenzaldehyde are heated under reflux in 65 ml of ethanol for 8 hours. The solvent is then evaporated, 15 ml of boiling methanol are added to the residue, the solution is discoloured with activated charcoal and cooled to -5° C. to obtain 2-(4-acetylaminobenzoyloxy)ethyl 2,6-dimethyl-5-ethoxycarbonyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylate with half a molecule of ethanol as yellow crystals melting--after recrystallisation in ehtanol--at 157°-162° C. The yield is 46% of the theoretical yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04727066 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-e8342923f9524540becdf8521b43cb93 |
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| 出典メモ | uspto-grants-1988_02 |
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