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Diisopropylether hexane → 2-Aminocarbonyloxymethyl-6-methyl-4-(3-nitrophenyl)-3-ethoxycarbonyl-5-(beta-ethoxyethoxy)carbonyl-1,4-dihydropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylether hexane | HCID 21881879 | — |
| 反応物 | 2-Ethoxyethyl 2-[(3-nitrophenyl)methylidene]-3-oxobutanoate | HCID 54574563 | — |
| 反応物 | Ethyl 4-carbamoyloxy-3-aminocrotonate | HCID 86742112 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-Aminocarbonyloxymethyl-6-methyl-4-(3-nitrophenyl)-3-ethoxycarbonyl-5-(beta-ethoxyethoxy)carbonyl-1,4-dihydropyridine | HCID 13092116 | 54% |
反応手順
9.4 g (50 millimoles) of ethyl 4-carbamoyloxy-3-aminocrotonate and 15.4 g (50 millimoles) of β-ethoxyethyl 2-(m-nitrobenzylidene)acetoacetate were dissolved in 200 ml of isopropyl alcohol and reacted at a temperature of from 60° to 70° C. for 18 hours. The reaction mixture was concentrated under reduced pressure. The residue was crystallized from diisopropylether-hexane, whereby 12 g (yield: 54%) of 2-carbamoyloxymethyl-6-methyl-4-(m-nitrophenyl)-3-ethoxycarbonyl-5-(β-ethoxyethoxy)carbonyl-1,4-dihydropyridine in crystal form was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04739106 |
| 出典データセット | uspto-grants-1988_04 |
| ORD ID | ord-4f826bf69c1f421caf8e499aa1994918 |
| 出典メモ | uspto-grants-1988_04 |