HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-(Trifluoromethyl)phenol → 2-(Methylsulfanyl)-4-(trifluoromethyl)-6-[3-(trifluoromethyl)phenoxy]pyrimidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 4-Chloro-2-(methylsulfanyl)-6-(trifluoromethyl)pyrimidine | HCID 248063 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 2-(Methylsulfanyl)-4-(trifluoromethyl)-6-[3-(trifluoromethyl)phenoxy]pyrimidine | HCID 1475000 | — |
Reaktionsschritte
m-(Trifluoromethyl)phenol (1.06 g, 0.0044×1.5 mol) and NaH (0.26 g (ca.60% in mineral oil), 0.0044×1.5 mol) were dissolved in THF, and then 4-chloro-2-methylthio-6-(trifluoromethyl)pyrimidine (Compound No. VII-17) (1.0 g, 0.0044 mol) was added thereto. The resulting solution was refluxed for about 7 hours. The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate to separate an organic phase. The organic phase was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated. Thereafter, remaining phenol and others were distilled off in a tubular oven (under water flow, 150° C.) to obtain the intermediate compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05723412 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-779700042b074f55b42f3a2202e7c555 |
| Quellennotiz | uspto-grants-1998_03 |