HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Nitrobenzaldehyde → Diethyl 1,2,3,4-tetrahydro-2-hydroxy-6-methyl-4-(3-nitrophenyl)-2-(trifluoromethyl)-3,5-pyridine-dicarboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Nitrobenzaldehyde | HCID 7449 | — |
| Edukt | Ethyl 4,4,4-trifluoroacetoacetate | HCID 67793 | — |
| Edukt | 2-Butenoic acid, 3-amino-, ethyl ester | HCID 95308 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | Diethyl 1,2,3,4-tetrahydro-2-hydroxy-6-methyl-4-(3-nitrophenyl)-2-(trifluoromethyl)-3,5-pyridine-dicarboxylate | HCID 20189336 | 21,3% |
Reaktionsschritte
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°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04686217 |
| Quelldatensatz | uspto-grants-1987_08 |
| ORD ID | ord-4363dabc83874b53a061e880dad7c775 |
| Quellennotiz | uspto-grants-1987_08 |