HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 1,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]-
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Methanol | HCID 887 | — |
| Edukt | Ethyl trifluoroacetate | HCID 9794 | — |
| Edukt | 1-(4-(Methylthio)phenyl)ethan-1-one | HCID 74501 | — |
| Edukt | Sodium Methoxide | HCID 10942334 | — |
| Lösungsmittel | tert-Butyl methyl ether | HCID 15413 | — |
| Produkt | 1,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]- | HCID 10730170 | 71% |
Reaktionsschritte
To a solution of ethyl trifluoroacetate (7.95 ml, 1.1 eq) in MTBE (125 ml) was added dropwise 25% sodium methoxide in methanol (16 ml, 1.2 eq). 4-Methylthioacetophenone (Aldrich, 10 g, 0.06 mol) was added portionwise and the mixture stirred at ambient temperature overnight. 2N Hydrochloric acid (40 ml) was added cautiously and the organic phase separated, washed with brine and dried (Na2SO4) to give an orange solid. The orange solid was recrystallised from hot isopropanol to give the title compound as a yellow crystalline solid (11.25 g, 71%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07084148B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-697eb1beb35a4059a73112f3071f16a1 |
| Quellennotiz | uspto-grants-2006_08 |