HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl (+/-)-3-methyl-1-trichloromethyl-2-butenyl diazomalonate → Ethyl (+/-)-4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo-[3.1.0]hexane-1-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl (+/-)-3-methyl-1-trichloromethyl-2-butenyl diazomalonate | HCID 53929412 | — |
| Katalysator | Copper | HCID 23978 | — |
| Lösungsmittel | Octane | HCID 356 | — |
| Produkt | Ethyl (+/-)-4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo-[3.1.0]hexane-1-carboxylate | HCID 12525249 | — |
Reaktionsschritte
To a refluxing suspension of copper powder (5.0 g, 0.079 mole) in 240 ml of n-octane was added dropwise in one hour a solution of ethyl (±)-3-methyl-1-trichloromethyl-2-butenyl diazomalonate (5.0 g, 0.0146 mole) in 60 ml of n-octane. The reaction mixture was then heated under reflux for 21/2 hours and filtered. The n-octane was removed from the filtrate by evaporation under vacuum, yielding a residue which was distilled under vacuum to give ethyl (±)-4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo-[3.1.0]hexane-1-carboxylate as a highly viscous oil (2.47 g, 54% yield); bp, 123°-125°/0.3 mm.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04254282 |
| Quelldatensatz | uspto-grants-1981_03 |
| ORD ID | ord-ccd1b7912f6b421a96814214cccc1cee |
| Quellennotiz | uspto-grants-1981_03 |