HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Carbonate → trans-3,7-dimethylhexahydro-1H-azepine-2-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | trans-2,6-Dimethylcyclohexanone oxime | HCID 40531046 | — |
| Lösungsmittel | O-Xylene | HCID 7237 | — |
| Produkt | trans-3,7-dimethylhexahydro-1H-azepine-2-one | HCID 66594919 | — |
Reaktionsschritte
Into 20 ml of xylene were added 1.3 g of trans-2,6-dimethylcyclohexanone oxime and 6 g of polyphosphoric acid, the mixture was stirred for 10 hours at 100%. The reaction mixture was cooled to near room temperature, poured into ice-water. Sodium carbonate was added to the mixture, and the mixture was extracted with ethyl acetate three times. The organic layers was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 1.2 g of trans-3,7-dimethylhexahydro-1H-azepine-2-one.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07732448B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-7aec735a879148f49e91979006a0a2c6 |
| Quellennotiz | uspto-grants-2010_06 |