HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cyclopropyl methyl ketone → 1-Cyclopropyl-3-(2-methylthio-4-trifluoromethylphenyl)-1,3-propanedione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cyclopropyl methyl ketone | HCID 13004 | — |
| Edukt | Sodium Methoxide | HCID 10942334 | — |
| Edukt | Methyl 2-(methylthio)-4-(trifluoromethyl)benzoate | HCID 10944828 | — |
| Lösungsmittel | Chlorobenzene | HCID 7964 | — |
| Produkt | 1-Cyclopropyl-3-(2-methylthio-4-trifluoromethylphenyl)-1,3-propanedione | HCID 11120178 | 99,3% |
Reaktionsbedingungen
| Temperatur | 75 °C |
|---|
Reaktionsschritte
Sodium methoxide (64 g, 1.15M) was added to a mixture of methyl 2-methylthio-4-trifluoromethylbenzoate (200 g, 0.8M) in chlorobenzene (380 g). The mixture was heated to 75° C. and cyclopropyl methyl ketone (75 g, 0.88M) added during 2 hours whilst maintaining stirring at 75° C. After 4 hours methanol was distilled under reduced pressure. the mixture cooled to 50° C., and water followed by sulphuric acid (53 g of 36N) added. The organic phase was distilled under reduced pressure to give 1-cyclopropyl-3-(2-methylthio-4-trifluoromethylphenyl)propane-1,3-dione as yellow crystals (240 g), m.p. 58-60° C. A yield of 88% was obtained. The purity of the product was 90%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06486356B2 |
| Quelldatensatz | uspto-grants-2002_11 |
| ORD ID | ord-bf69f87a0bd1485ab4273d94effa8768 |
| Quellennotiz | uspto-grants-2002_11 |