HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → Ethyl 4-chloro-1-{[4-(methyloxy)phenyl]methyl}-1H-pyrrolo[3,2-c]pyridine-7-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Phosphorodichloridic acid, phenyl ester | HCID 13038 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | Ethyl 1-{[4-(methyloxy)phenyl]methyl}-4-oxo-4,5-dihydro-1H-pyrrolo[3,2-c]pyridine-7-carboxylate | HCID 57840819 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | Ethyl 4-chloro-1-{[4-(methyloxy)phenyl]methyl}-1H-pyrrolo[3,2-c]pyridine-7-carboxylate | HCID 57840887 | — |
Reaktionsschritte
Ethyl 1-{[4-(methyloxy)phenyl]methyl}-4-oxo-4,5-dihydro-1H-pyrrolo[3,2-c]pyridine-7-carboxylate (2.90 g) and phenyl dichlorophosphate (18 ml) were heated at 180° C. under argon for 30 minutes. The reaction mixture was allowed to cool, poured onto iced water, and neutralised to pH7 using solid sodium bicarbonate. To the reaction mixture was added ethyl acetate and the insoluble material was filtered off. The aqueous was separated and extracted three times with ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4), filtered and evaporated to afford the title compound as a clear oil (2.0 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07589206B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-73ad1c02fc9a4848ad7456417a31f865 |
| Quellennotiz | uspto-grants-2009_09 |