S-(3-triethoxysilylpropyl) octanethioate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 1,021 grams of 3-mercaptopropyltriethoxysilane (SILQUEST® A-1891 silane from OSi Specialties, Inc., a subsidiary of Crompton Corp. of Greenwich, Conn.), 433 grams of triethylamine, and 3,000 ml hexane. The solution was cooled in an ice bath, and 693 grams of octanoyl chloride were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent. Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel The solution was cooled in an ice bath the mixture was filtered two times first through a 0.1 μm filter through a 0.01 μm filter filter to remove the salt The solvent was removed under vacuum distilled

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

実験手順: Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 3-mercaptopropyltriethoxysilane (1,021 grams, 3.73 moles purchase as SILQUEST® A-1891 silane from General Electric Company), triethylamine (433 grams), and hexane (3,000 ml). The solution was cooled in an ice bath, and octanoyl chloride (693 grams, 4.25 moles) were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent. Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel The solution was cooled in an ice bath the mixture was filtered two times first through a 0.1 μm filter through a 0.01 μm filter filter to remove the salt The solvent was removed under vacuum distilled

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

実験手順: Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 3-mercaptopropyltriethoxysilane (1,021 grams, 3.73 moles purchase as SILQUEST® A-1891 silane from General Electric Company), triethylamine (433 grams), and hexane (3,000 ml). The solution was cooled in an ice bath, and octanoyl chloride (693 grams, 4.25 moles) were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent. Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel The solution was cooled in an ice bath the mixture was filtered two times first through a 0.1 μm filter through a 0.01 μm filter filter to remove the salt The solvent was removed under vacuum distilled

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

実験手順: Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 3-mercaptopropyltriethoxysilane (1,021 grams, 3.73 moles purchase as SILQUEST® A-1891 silane from General Electric Company), triethylamine (433 grams), and hexane (3,000 ml). The solution was cooled in an ice bath, and octanoyl chloride (693 grams, 4.25 moles) were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent. Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel The solution was cooled in an ice bath the mixture was filtered two times first through a 0.1 μm filter through a 0.01 μm filter filter to remove the salt The solvent was removed under vacuum distilled

反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The aqueous solution of sodium thiooctanoate was heated to 40° C. and 11 grams of 34.5% HEGCl solution were added. Also, about 296 grams of 3-chloro-1-propyltriethoxysilane were added batch-wise to the reaction mixture. The product was heated further to 90° C. and stirred for 5 hours. At this point, agitation was discontinued and the two-phase system was allowed to separate. The bottom aqueous phase was removed and the top crude product was recovered. The crude layer was purified by stripping the material at 135-145° C. and 5-10 mm Hg. The process yielded about 251 grams of pale yellow and clear product with a typical GC purity of 92-94%. 11 grams of 34.5% HEGCl solution were added to separate The bottom aqueous phase was removed the top crude product was recovered The crude layer was purified at 135-145° C. The process yielded about 251 grams of pale yellow and clear product with a typical GC purity of 92-94%

反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The aqueous solution of sodium thiooctanoate was heated to 40° C. and 11 grams of 34.5% HEGCl solution were added. Also, about 296 grams of 3-chloro-1-propyltriethoxysilane were added batch-wise to the reaction mixture. The product was heated further to 90° C. and stirred for 5 hours. At this point, agitation was discontinued and the two-phase system was allowed to separate. The bottom aqueous phase was removed and the top crude product was recovered. The crude layer was purified by stripping the material at 135-145° C. and 5-10 mm Hg. The process yielded about 251 grams of pale yellow and clear product with a typical GC purity of 92-94%. 11 grams of 34.5% HEGCl solution were added to separate The bottom aqueous phase was removed the top crude product was recovered The crude layer was purified at 135-145° C. The process yielded about 251 grams of pale yellow and clear product with a typical GC purity of 92-94%

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

実験手順: Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 1,021 grams of 3-mercaptopropyltriethoxysilane (SILQUEST® A-1891 silane from OSi Specialties, Inc., a subsidiary of Crompton Corp. of Greenwich, Conn.), 433 grams of triethylamine, and 3,000 ml hexane. The solution was cooled in an ice bath, and 693 grams of octanoyl chloride were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent. Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel The solution was cooled in an ice bath the mixture was filtered two times first through a 0.1 μm filter through a 0.01 μm filter filter to remove the salt The solvent was removed under vacuum distilled

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

実験手順: Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 3-mercaptopropyltriethoxysilane (1,021 grams, 3.73 moles purchase as SILQUEST® A-1891 silane from General Electric Company), triethylamine (433 grams), and hexane (3,000 ml). The solution was cooled in an ice bath, and octanoyl chloride (693 grams, 4.25 moles) were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent. Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel The solution was cooled in an ice bath the mixture was filtered two times first through a 0.1 μm filter through a 0.01 μm filter filter to remove the salt The solvent was removed under vacuum distilled

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

実験手順: Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 3-mercaptopropyltriethoxysilane (1,021 grams, 3.73 moles purchase as SILQUEST® A-1891 silane from Momentive Performance Materials, Inc.), triethylamine (433 grams), and hexane (3,000 ml). The solution was cooled in an ice bath, and octanoyl chloride (693 grams, 4.25 moles) were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent. Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel The solution was cooled in an ice bath the mixture was filtered two times first through a 0.1 μm filter through a 0.01 μm filter filter to remove the salt The solvent was removed under vacuum distilled