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3-Nitrobenzaldehyde → Diethyl 1,2,3,4-tetrahydro-2-hydroxy-6-methyl-4-(3-nitrophenyl)-2-(trifluoromethyl)-3,5-pyridine-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Nitrobenzaldehyde | HCID 7449 | — |
| 反応物 | Ethyl 4,4,4-trifluoroacetoacetate | HCID 67793 | — |
| 反応物 | 2-Butenoic acid, 3-amino-, ethyl ester | HCID 95308 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Diethyl 1,2,3,4-tetrahydro-2-hydroxy-6-methyl-4-(3-nitrophenyl)-2-(trifluoromethyl)-3,5-pyridine-dicarboxylate | HCID 20189336 | 21.3% |
反応手順
3-Nitrobenzaldehyde (3.0 g, 20 mmoles), ethyl 3-amino-2-butenoate (2.6 g, 20 mmoles) and ethyl 4,4,4-trifluoro-3-oxobutanoate (2.92 ml, 20 mmoles) were heated at reflux in ethanol (25 ml) for 6 hours. The solvent was removed in vacuo and the residue crystallised by the addition of ether/petroleum ether (60°-80°). The resulting solid was recrystallised from ether/petroleum ether (60°-80°) to give the title compound as colourless crystals (1.9 g) mp 120°-1°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04607041 |
| 出典データセット | uspto-grants-1986_08 |
| ORD ID | ord-06f20a5dd9a44b7abc75750ac250ae5c |
| 出典メモ | uspto-grants-1986_08 |