Toluene → p-Chlorophenyldimethylvinylsilane

HRID 1448444Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1448444
[CH3:1][Si:2]([CH3:5])(Cl)Cl.[C:6]1(C)[CH:11]=CC=C[CH:7]=1.[Cl:13][C:14]1[CH:19]=[CH:18]C([Mg]Cl)=[CH:16][CH:15]=1.C([Mg]Cl)=C>O1CCCC1>[Cl:13][C:14]1[CH:15]=[CH:16][C:1]([SiH2:2][CH:5]=[C:6]([CH3:11])[CH3:7])=[CH:18][CH:19]=1

Komponenten

6

Edukt 4

HCID 1140Toluene2×HCID 6398DichlorodimethylsilaneHCID 178461836HCID 178461836, VerbindungHCID 178478983HCID 178478983, Verbindung

Produkt 1

HCID 131711671p-ChlorophenyldimethylvinylsilaneAusbeute 51,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Forty cubic centimeters (0.33 mol) of dimethyldichloro silane at 20° C. were placed in a 3-neck balloon-flask swept by a flow of nitrogen. Eighty cubic centimeters of toluene were added while shaking the mixture. The temperature was reduced to 5° C., then 0.33 mol of p-chlorophenylmagnesium chloride in 30 mn in the form of a solution in tetrahydrofurane (140 cubic centimeters) were added. Twenty cubic centimeters of toluene were added and the mixture was shaken for 2 hours 30 minutes. Then, 0.36 mol of vinylmagnesium chloride at 20 mn in the form of a solution in tetrahydrofurane (120 cubic centimeters) were added, the temperature being 25° C. at that time. Then the temperature of the reactive environment was changed and maintained for 2 hours. The reactive environment was cooled, the mixture was washed twice with 100 cubic centimeters of water, acidified with 5 cubic centimeters of HCl. Then, after decantation, the mixture was neutralized by means of sodium bicarbonate, dried, and 42 grams of a product containing (chromatography in the gaseous phase) 80 percent in terms of weight of p-chlorophenyldimethylvinylsilane (yield of 51.3 percent as compared to dimethylchlorosilane) was collected.

Aufarbeitung

  1. customwas reduced to 5° C.
  2. stirringthe mixture was shaken for 2 hours 30 minutes
  3. custombeing 25° C. at that time
  4. temperaturemaintained for 2 hours
  5. temperatureThe reactive environment was cooled
  6. washthe mixture was washed twice with 100 cubic centimeters of water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d17e7aa297d7450086d97ca2a1839b87
Quelldatensatz
uspto-grants-1979_12
Patentnummer
US04180515

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