Reaktion #346141

Reaktionsgleichung

p-Methoxystyrene

1,1-dichloro-2,2-difluoroethylene

triethylamine

→

2,2-Dichloro-1,1-difluoro-3-(p-methoxyphenyl)cyclobutane

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe reaction product extracted with ether
2. 2
   Waschenthe extracts washed with water
3. 3
   Trocknendried (MgSO4)
4. 4
   Sonstigeevaporated to an oil
5. 5
   workup.DISTILLATIONDistillation of the oil
6. 6
   Sonstigeyields 69.0 g
7. 7
   SonstigePart of the oil was chromatographed (alumina, cyclohexane)
8. 8
   workup.DISTILLATIONredistilled

Vorschrift

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.

Quelle