Reaktion #963284

Reaktionsgleichung

benzoyl isothiocyanate

3-aminopropyl trimethoxysilane

→

Benzoyl Thiourea Propyltrimethoxysilane

Ausbeute 97.0%

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 250 mL 3-neck RBF equipped with a condenser, magnetic stirrer
2. 2
   Sonstigethermo-probe, nitrogen purge
3. 3
   workup.ADDITIONwere added slowly over a period of time of 30 minutes
4. 4
   SonstigeThe ice-water bath was removed
5. 5
   Sonstigepurge overnight
6. 6
   EinengenThe reaction mixture was then concentrated in vacuo at a temperature of 40° C.
7. 7
   Sonstigeto provide a clear red liquid
8. 8
   SonstigeThe liquid was dried to constant weight in vacuo at a temperature of 50° C.

Vorschrift

To a 250 mL 3-neck RBF equipped with a condenser, magnetic stirrer, thermo-probe, nitrogen purge and pressure-equilibrated addition funnel was added benzoyl isothiocyanate (25.0 g, 0.150 mol) followed by dichloromethane (100 mL). The reaction mixture was cooled in an ice-water bath to a temperature below 5° C., at which point 3-aminopropyl trimethoxysilane (27.7 g, 0.150 mol) and dichloromethane (100 mL) were added slowly over a period of time of 30 minutes. The ice-water bath was removed and the reaction mixture was stirred at room temperature under a nitrogen purge overnight. The reaction mixture was then concentrated in vacuo at a temperature of 40° C. to provide a clear red liquid. The liquid was dried to constant weight in vacuo at a temperature of 50° C. and a pressure of <1 mTorr in a 97% yield.

Quelle