1,1-Dichloro-2,2-difluoroethene → Benzene, 1-(2,2-dichloro-3,3-difluorocyclobutyl)-4-methoxy-

HRID 1578800

Reaktionsgleichung

Reaktionsgleichung von HRID 1578800
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[CH2:8])=[CH:5][CH:4]=1.[Cl:11][C:12]([Cl:16])=[C:13]([F:15])[F:14].C(N(CC)CC)C>O>[Cl:11][C:12]1([Cl:16])[CH:7]([C:6]2[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH2:8][C:13]1([F:15])[F:14]

Komponenten

5

Edukt 3

HCID 65921,1-Dichloro-2,2-difluoroetheneHCID 8471TriethylamineHCID 125074-Methoxystyrene

Produkt 1

HCID 21425195Benzene, 1-(2,2-dichloro-3,3-difluorocyclobutyl)-4-methoxy-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

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 suitable 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.

Aufarbeitung

  1. extractionthe reaction product extracted with ether
  2. washthe extracts washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated to an oil
  5. distillationDistillation of the oil
  6. customyields 69.0 g
  7. customPart of the oil was chromatographed (alumina, cyclohexane)
  8. distillationredistilled

Quellen und Nachweise

ORD-Eintrag
ord-7f4063ac18d74b2fa4f79215acf6d0f0
Quelldatensatz
uspto-grants-1976_02
Patentnummer
US03939196

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