Reaktion #1112424

Reaktionsgleichung

N,N-dimethylcarbamoyl chloride

triethylamine

3-aminopropyltrimethoxysilane

→

silane

Ausbeute 82.5%

1,1-dimethyl-3-(3-(trimethoxysilyl)propyl)urea

Ausbeute 82.5%

Lösungsmittel

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with a reflux cooler
2. 2
   SonstigeAfter the exothermic reaction
3. 3
   workup.STIRRINGthe resulting whitish suspension was stirred at 90° C. for 3 hours
4. 4
   Sonstigethe solid was separated by double filtration
5. 5
   Sonstigethe solvent was removed at 60° C. for 1 hour on a rotary evaporator

Vorschrift

5.0 g (46.5 mmol) N,N-dimethylcarbamoyl chloride (Sigma-Aldrich, Switzerland) and 40 ml, dried dioxane (Sigma-Aldrich, Switzerland) were added to a 250-mL round-bottom two-neck flask equipped with a reflux cooler. 4.71 g (46.5 mmol) triethylamine (Sigma-Aldrich, Switzerland) and 8.34 g (46.5 mmol) 3-aminopropyltrimethoxysilane (Silquest A-1110, Momentive Performance Materials Inc., USA) were added dropwise under nitrogen, with stirring. After the exothermic reaction subsided, the resulting whitish suspension was stirred at 90° C. for 3 hours. A gradual color change to orange was observed. After cooling to 50° C., the solid was separated by double filtration, and the solvent was removed at 60° C. for 1 hour on a rotary evaporator. 9.6 g of the desired silane was obtained as a brown liquid. The silane was designated as DMA1100 and used without further purification.

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