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-

HRID 268104Notes

Reaction equation

HRID 268104 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

Reactant 2

HCID 925063,14-Dioxa-8,9-dithia-4,13-disilahexadecane, 4,4,13,13-tetraethoxy-HCID 5362487Sulfur3×

Product 1

HCID 925073,15-Dioxa-8,9,10-trithia-4,14-disilaheptadecane, 4,4,14,14-tetraethoxy-

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

  1. customdid not crystallize out again
  2. temperatureupon cooling
  3. customA dark red liquid was formed

Sources & evidence

ORD record
ord-e6617bb316af4baa8027c08180291e0f
Source dataset
uspto-grants-1976_03
Patent number
US03946059

Reaction notes

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