3,14-Dioxa-8,9-dithia-4,13-disilahexadecane, 4,4,13,13-tetraethoxy- → 3,15-Dioxa-8,9,10-trithia-4,14-disilaheptadecane, 4,4,14,14-tetraethoxy-
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]>>[CH2:15]([O:14][Si:13]([O:20][CH2:21][CH3:22])([O:17][CH2:18][CH3:19])[CH2:12][CH2:11][CH2:10][S:9][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])[CH3:16]Participants
3
Procedure
47.5 g of bis-[γ-(triethoxysilyl)-propyl]-disulfide (0.1 mole) was heated together with 3.2 g of sulfur (0.1 mole) under a nitrogen gas atmosphere for about 15 hours at about 150°C, until all of the sulfur had dissolved and did not crystallize out again upon cooling. A dark red liquid was formed, which a thin-layer chromatogram showed to contain no free sulfur, and in which disulfides and tetrasulfides are dissolved as shown by mass spectrographic analysis.
Workup
- customdid not crystallize out again
- temperature