Reaktion #624901

Reaktionsgleichung

tetrahydrothiophene

trimethoxysilylpropyl iodide

→

trimethoxysilylpropyltetrahydrothiophene iodide

Lösungsmittel

ethyl acetate

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONto be dissolved
2. 2
   workup.ADDITIONmixed solution with a magnetic stirrer
3. 3
   workup.ADDITIONwas gradually added at room temperature in a nitrogen atmosphere
4. 4
   TemperaturThe reaction mixture was refluxed over 3 days
5. 5
   workup.DISTILLATIONethyl acetate was distilled off under reduced pressure
6. 6
   EinengenThe resultant concentrate
7. 7
   workup.ADDITIONwas dropped into 100 mL of diethyl ether
8. 8
   Sonstigetetrahydrothiophene and trimethoxysilylpropyl iodide as by-products were removed
9. 9
   SonstigeThis purification
10. 10
    workup.DISTILLATIONremaining diethyl ether was distilled off under reduced pressure
11. 11
    workup.DISSOLUTIONby dissolving the resultant
12. 12
    Einengenconcentrate in methanol

Vorschrift

2.0 g of tetrahydrothiophene and 18 g of ethyl acetate were charged into a 100 mL flask to be dissolved. While stirring the resultant mixed solution with a magnetic stirrer, to the mixed solution, a solution in which 9.9 g of trimethoxysilylpropyl iodide was dissolved in 24 g of ethyl acetate was gradually added at room temperature in a nitrogen atmosphere. The reaction mixture was refluxed over 3 days and therefrom, ethyl acetate was distilled off under reduced pressure. The resultant concentrate was dropped into 100 mL of diethyl ether and therefrom, tetrahydrothiophene and trimethoxysilylpropyl iodide as by-products were removed. This purification was repeated three times and then remaining diethyl ether was distilled off under reduced pressure, followed by dissolving the resultant concentrate in methanol to obtain a 30% methanol solution of trimethoxysilylpropyltetrahydrothiophene iodide.

Quelle