HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → HCID 57618621, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Trifluoroacetic acid | HCID 6422 | — |
| Edukt | 5-Acetyl-7a-pyrrolidin-1-yl-3a,4,5,6,7,7a-hexahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester | HCID 57618619 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 57618621 | HCID 57618621 | — |
Reaktionsschritte
A mixture of 18.0 g (58 mmol) of 5-acetyl-7a-pyrrolidin-1-yl-3a,4,5,6,7,7a-hexahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester (B) in 150 mL of DCM and 6.47 mL (87 mmol) of trifluoroacetic acid was heated to reflux for 8 h. After addition of 100 mL of water, the organic phase was dried over MgSO4 and the solvent removed under a vacuum. The remaining brown oil was purified by column chromatography (SiO2, EtOAc/EtOH 10:1). 12.5 g (90% of theoretical) of the desired product 5-acetyl-4,5,6,7-tetrahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester (C) were obtained in the form of a brown-yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08048879B2 |
| Quelldatensatz | uspto-grants-2011_11 |
| ORD ID | ord-1345c9612dcd45efb79401cc3bce7f0b |
| Quellennotiz | uspto-grants-2011_11 |