triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 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. did not crystallize out again when the solution was cooled A dark red, viscous solution was formed

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 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. did not crystallize out again when the solution was cooled A dark red, viscous solution was formed

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 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. did not crystallize out again when the solution was cooled A dark red, viscous solution was formed

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 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. did not crystallize out again when the solution was cooled A dark red, viscous solution was formed