Reaktion #58788

ord-3994d8fbc2414735b1726cfcc0b8241d

Lösungsmittel

Reaktionsbedingungen

Temperatur
105°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONis distilled off in vacuo at 15-600 mbar
  2. 2
    TemperaturAfter cooling
  3. 3
    Sonstige7022 g of a colourless, solid product are obtained

Vorschrift

2002.6 g of 3-mercaptopropyl(triethoxy)silane are mixed with 6108.5 g of hexadecanol as well as with 2 g of tetrabutyl orthotitanate and heated at 95-115° C. for 360 minutes in a 10 liter flask in a distillation apparatus. Ethanol formed in the transesterification is distilled off in vacuo at 15-600 mbar. After cooling, 7022 g of a colourless, solid product are obtained. As can be shown by 1H-NMR and 29Si-NMR, 92% of the EtO—Si groups are replaced by R—O—Si. In the transesterification more than 80 mole % of the ethanol-free compound [(C16H33O)3Si—C3H6—SH is formed, as can be shown for example by 1H-NMR and 29Si-NMR.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07423165B2uspto-grants-2008_09