반응 #963284

반응 방정식

benzoyl isothiocyanate

3-aminopropyl trimethoxysilane

→

Benzoyl Thiourea Propyltrimethoxysilane

수율 97.0%

용매

dichloromethane

dichloromethane

반응 조건

후처리

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

실험 절차

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.

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