HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Gamma-Butyrolactone → 1,3-Dioxo-6-hydroxy-1(3'-tert-butyl-phenyl)-hexane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Gamma-Butyrolactone | HCID 7302 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | 1-(3-tert-Butylphenyl)ethan-1-one | HCID 13657978 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | 1,3-Dioxo-6-hydroxy-1(3'-tert-butyl-phenyl)-hexane | HCID 57839120 | — |
Reaktionsschritte
To a stirring suspension of NaH (60% in oil, 7.66 g) in ether (480 ml) at 0° C. was added ethanol (479 μL), followed by γ-butyrolactone (6.18 ml). This was followed by dropwise addition of 1-(3-tert-butyl-phenyl)-ethanone (13.5 g) in ether (80 ml). The resulting mixture was allowed to warm to room temperature and stirred for 72 hours. After careful addition of ethanol (10.5 ml), ammonium chloride solution (10 g in 250 ml water) was then added, ether layer was then separated and washed with brine (300 ml), dried over MgSO4 and concentrated in vacuo to give 1,3-dioxo-6-hydroxy-1(3′-tert-butyl-phenyl)-hexane as crude product (18.5 g). This required no purification and was immediately used in the next reaction.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07589095B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-44a0741dc5894e7abf0078fe50f4a301 |
| Quellennotiz | uspto-grants-2009_09 |