Vinyltrichlorosilane → Vinyltris(furfuryloxy)silane

HRID 464620

Reaktionsgleichung

Reaktionsgleichung von HRID 464620
[CH2:1]([OH:7])[C:2]1[O:6][CH:5]=[CH:4][CH:3]=1.[Na].[CH:9]([Si:11](Cl)(Cl)Cl)=[CH2:10]>C1(C)C=CC=CC=1>[CH:9]([Si:11]([O:7][CH2:1][C:2]1[O:6][CH:5]=[CH:4][CH:3]=1)([O:7][CH2:1][C:2]1[O:6][CH:5]=[CH:4][CH:3]=1)[O:7][CH2:1][C:2]1[O:6][CH:5]=[CH:4][CH:3]=1)=[CH2:10]

Komponenten

5

Edukt 3

HCID 6413VinyltrichlorosilaneHCID 7361Furfuryl Alcohol2×HCID 5360545Sodium2×

Produkt 1

HCID 20262148Vinyltris(furfuryloxy)silane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of 86.5 ml. furfuryl alcohol in 200 ml. toluene was slowly added 23 g. sodium metal. An additional 10 ml. furfuryl alcohol was added and the solution was heated to 100° C. with stirring to convert all the sodium. The solution was cooled to ice temperature and 43.5 ml. vinyltrichlorosilane dissolved in 50 ml. toluene was slowly added. After the addition was complete, the mixture was heated at 95° C. for 0.5 hr. The colloidal sodium chloride by-product was extracted with water. The organic phase was filtered and the toluene removed by vacuum evaporation. The residue was distilled at 2 mmHg and the product recovered at 182°-184° C.

Aufarbeitung

  1. temperatureThe solution was cooled to ice temperature and 43.5 ml
  2. additionAfter the addition
  3. temperaturethe mixture was heated at 95° C. for 0.5 hr
  4. extractionThe colloidal sodium chloride by-product was extracted with water
  5. filtrationThe organic phase was filtered
  6. customthe toluene removed by vacuum evaporation
  7. distillationThe residue was distilled at 2 mmHg
  8. customthe product recovered at 182°-184° C.

Quellen und Nachweise

ORD-Eintrag
ord-5735451fbb0543139db59cf91f9862f3
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04548865

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