Hydrogen Sulfide → (3-Mercaptopropyl)trimethoxysilane

HRID 357672

Reaktionsgleichung

Reaktionsgleichung von HRID 357672
[SH2:1].Cl[CH2:3][CH2:4][CH2:5][Si:6]([O:11][CH3:12])([O:9][CH3:10])[O:7][CH3:8]>CO>[SH:1][CH2:3][CH2:4][CH2:5][Si:6]([O:11][CH3:12])([O:9][CH3:10])[O:7][CH3:8]

Komponenten

4

Edukt 2

HCID 402Hydrogen Sulfide3×HCID 624493-(Trimethoxysilyl)propyl chloride

Produkt 1

HCID 20473(3-Mercaptopropyl)trimethoxysilaneAusbeute 93,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

267.6 g of a methanol solution of 22% sodium hydrogensulfide anhydride (1.05 mol) was put into an autoclave with an internal volume of 1 liter and the air was replaced by nitrogen. 0.3 mol of hydrogen sulfide was then blown in and the system was pressurized to 0.9 kgf/cm2 to oversaturate hydrogen sulfide. After heating the system up to 90° C., 198.7 g (1.0 mole) of 3-chloropropyltrimethoxy silane was dripped for 3 hours, and during the dripping, 0.1 mol of hydrogen sulfide was blown into the system so that the pressure in the system was kept at 3.5 kgf/cm2. After the dripping, the system was aged for 2 hour at 90° C., followed by cooling. By-product salts produced in the reaction were filtered away. The composition was analyzed by means of gas chromatography. 3-mercaptopropyltrimethoxy silane was obtained with a yield of 93.5%.

Aufarbeitung

  1. temperatureby cooling
  2. customBy-product salts produced in the reaction
  3. filtrationwere filtered away

Quellen und Nachweise

ORD-Eintrag
ord-831230018a3848bc86430b5f919e4fbc
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05840952

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