HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,1-Dichloro-2,2-difluoroethene → Benzene, 1-(2,2-dichloro-3,3-difluorocyclobutyl)-4-methoxy-
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,1-Dichloro-2,2-difluoroethene | HCID 6592 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 4-Methoxystyrene | HCID 12507 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | Benzene, 1-(2,2-dichloro-3,3-difluorocyclobutyl)-4-methoxy- | HCID 21425195 | — |
Reaktionsschritte
p-Methoxystyrene (40.8 g., 0.30 mole), 1,1-dichloro-2,2-difluoroethylene (55.8 g., 0.42 mole), and triethylamine (3.0 ml., 0.02 mole) are heated in a sealed tube (25 × 615 mm) at 125°-130° C. for 16 hrs. The cooled mixture is then poured into water, the reaction product extracted with ether, and the extracts washed with water, dried (MgSO4), and evaporated to an oil. Distillation of the oil yields 69.0 g. (86%), b.p. 80°-85° C. (0.1 mm), of the desired intermediate sutiable for use in the next step. Part of the oil was chromatographed (alumina, cyclohexane), and redistilled, b.p. 81° C. (0.02 mm), nD27 1.5207.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04035426 |
| Quelldatensatz | uspto-grants-1977_07 |
| ORD ID | ord-38d988b8ebe3450c9217832735ceadc0 |
| Quellennotiz | uspto-grants-1977_07 |