3,14-Dioxa-8,9-dithia-4,13-disilahexadecane, 4,4,13,13-tetraethoxy- → 4,4,15,15-Tetraethoxy-3,16-dioxa-8,9,10,11-tetrathia-4,15-disilaoctadecane
Reaction equation
C(O[Si](OCC)(OCC)CCC[S:8][S:9][CH2:10][CH2:11][CH2:12][Si:13]([O:20][CH2:21][CH3:22])([O:17][CH2:18][CH3:19])[O:14][CH2:15][CH3:16])C.[S]>>[CH2:21]([O:20][Si:13]([O:17][CH2:18][CH3:19])([O:14][CH2:15][CH3:16])[CH2:12][CH2:11][CH2:10][S:9][S:8][S:8][S:9][CH2:10][CH2:11][CH2:12][Si:13]([O:14][CH2:15][CH3:16])([O:17][CH2:18][CH3:19])[O:20][CH2:21][CH3:22])[CH3:22]Participants
3
Procedure
47.5 g of bis-[γ-(triethoxysilyl)-propyl]-disulfide (0.1 mole) was heated together with 6.2 g of sulfur (0.2 mole) in a nitrogen gas atmosphere for about 50 hours at 160°C, until all of the sulfur had gone into solution and did not crystallize out again when the solution was cooled. A dark red, viscous solution was formed, which a thin-layer chromatograph shows to contain no more free sulfur, and which, according to mass spectrometric analysis, contains a small amount of pentasulfide in addition to disulfides and trisulfides.
Workup
- custom