triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)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 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. did not crystallize out again upon cooling A dark red liquid 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 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. did not crystallize out again upon cooling A dark red liquid was formed

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

実験手順: A mixture of 129 l of ethanol and 129 l of 3-chloropropyltriethoxysilane is placed in the reactor of comparison example 1. 13.85 kg of sulfur in the form of a powder are metered in. 35.6 kg of virtually anhydrous sodium sulfide is then added. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction. The reaction mixture is kept for a further 1.5 hours at 82-83° C. and then cooled. The reaction mixture is worked up as in comparison example 1. An almost water-white product is obtained. HPLC analysis confirms in this case too the presence of a polysulfane mixture with a mean chain length of 2, though the mixture has a high monosulfane content. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction cooled

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

実験手順: A mixture of 129 l of ethanol and 129 l of 3-chloropropyltriethoxysilane is placed in the reactor of comparison example 1. 13.85 kg of sulfur in the form of a powder are metered in. 35.6 kg of virtually anhydrous sodium sulfide is then added. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction. The reaction mixture is kept for a further 1.5 hours at 82-83° C. and then cooled. The reaction mixture is worked up as in comparison example 1. An almost water-white product is obtained. HPLC analysis confirms in this case too the presence of a polysulfane mixture with a mean chain length of 2, though the mixture has a high monosulfane content. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction cooled

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

実験手順: A mixture of 129 l of ethanol and 129 l of 3-chloropropyltriethoxysilane is placed in the reactor of comparison example 1. 13.85 kg of sulfur in the form of granules is metered in. 35.6 kg of virtually anhydrous sodium sulfide is then added. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction. The reaction mixture is kept for a further 1.5 hours at 82-83° C. and then cooled. The reaction mixture is worked up as in comparison example 1. An almost water-white product is obtained. HPLC analysis confirms in this case too the presence of a polysulfane mixture with a mean chain length of 2, though the mixture has a high monosulfane content. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction cooled

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

実験手順: A mixture of 129 l of ethanol and 129 l of 3-chloropropyltriethoxysilane is placed in the reactor of comparison example 1. 13.85 kg of sulfur in molten form is then metered in through a fine nozzle. 35.6 kg of virtually anhydrous sodium sulfide is then added. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction. The reaction mixture is kept for a further 1.5 hours at 82-83° C. and then cooled. The reaction mixture is worked up as in comparison example 1. An almost water-white product is obtained. HPLC analysis confirms in this case too the presence of a polysulfane mixture with a mean chain length of 2, though the mixture has a high monosulfane content. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction cooled

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

実験手順: A mixture of 129 l of ethanol and 129 l of 3-chloropropyltriethoxysilane is placed in the reactor of comparison example 1. 13.85 kg of sulfur in molten form is then metered in through a fine nozzle. 35.6 kg of virtually anhydrous sodium sulfide is then added. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction. The reaction mixture is kept for a further 1.5 hours at 82-83° C. and then cooled. The reaction mixture is worked up as in comparison example 1. An almost water-white product is obtained. HPLC analysis confirms in this case too the presence of a polysulfane mixture with a mean chain length of 2, though the mixture has a high monosulfane content. The temperature of the reactor contents rises to 82° C. on account of the exothermic reaction cooled

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 17.8 kg of virtually anhydrous sodium sulfide are mixed with 190 l of ethanol and added to an enameled 500 l capacity reactor. This is followed by the addition through a fine nozzle of 13.85 kg of sulfur in molten form. The mixture is heated to 50° C. and 190 l of 3-chloropropyltriethoxysilane are metered in within 10 minutes. On account of the exothermic reaction the temperature of the reactor contents rises to 74° C. A further 4.45 kg of virtually anhydrous sodium sulfide are added at this temperature. Three further portions of sodium sulfide are added at 5 minute intervals (i.e. each 5 minutes), the temperature of the reactor contents rising to 82° C. After completion of the sodium sulfide addition the reaction mixture is kept for 1.5 hours at 82-83° C. and the sodium chloride that has precipitated is separated after cooling the mixture. A yellow product is obtained after evaporating the reaction mixture in vacuo and renewed fine filtration. HPLC analysis confirms the presence of a product with a mean polysulfane chain length of 2. added to an enameled 500 l capacity reactor are metered in within 10 minutes On account of the exothermic reaction the temperature of the reactor contents rises to 74° C rising to 82° C the sodium chloride that has precipitated is separated after cooling the mixture A yellow product is obtained after evaporating the reaction mixture in vacuo filtration

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 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. did not crystallize out again upon cooling A dark red liquid was formed