HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfuric Acid → (S)-7-[(1,3-Dihydro-1,3-dioxo-2H-isoindol-2-yl)]-1,2,6,7,8,12b-hexahydro-6-oxopyrido[2,1-a][2]benzazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Trifluoroacetic anhydride | HCID 9845 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | (S)-N-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)-1-oxo-3-phenylpropyl]-1,4-dihydro-pyridine | HCID 15380836 | — |
| Lösungsmittel | Ethyl acetate hexane | HCID 21226206 | — |
| Produkt | (S)-7-[(1,3-Dihydro-1,3-dioxo-2H-isoindol-2-yl)]-1,2,6,7,8,12b-hexahydro-6-oxopyrido[2,1-a][2]benzazepine | HCID 9863597 | — |
Reaktionsschritte
Combine sulfuric acid (3.0 mL, 96%) and trifluoroacetic anhydride (300 mL). Add (S)-N-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)-1-oxo-3-phenylpropyl]-1,4-dihydro-pyridine (1.0 mmol). After 30 minutes, pour the reaction mixture into mixture of saturated aqueous sodium bicarbonate and ice. Extract with ethyl acetate and then with methylene chloride. Combine the organic layers and filter through a plug of silica gel. Rinse the silica gel with dichloromethane. Evaporate the filtrate in vacuo to give a residue. Chromatograph the residue on silica gel eluting sequentially with 10% ethyl acetate/hexane and then 25% ethyl acetate/hexane to give the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05859252 |
| Quelldatensatz | uspto-grants-1999_01 |
| ORD ID | ord-3c1672865aea43538351043f1ac29aa6 |
| Quellennotiz | uspto-grants-1999_01 |