反应详情

温度

55 °C

The aqueous solution of sodium thiooctanoate was heated to 50° C. and stirred with a mechanical stirrer throughout this procedure. To this solution was added, all at once, 0.21 grams of a concentrated aqueous solution of methyltrioctylammonium chloride. Immediately thereafter was added a solution of 3-chloro-1-propyltriethoxysilane (310 grams, 1.29 moles) in 23.6 grams of n-tetradecane. Over the next 15-20 minutes, the temperature of the contents of the 5-liter flask was increased to 55° C., with continued stirring. This temperature was then maintained for 5-6 hours, with continued stirring. The temperature was then ramped up to 70° C. over the next 7 minutes, and maintained for about another 2 hours, with continued stirring, whereupon the temperature was raised to and subsequently maintained at 78° C. for an additional 24 hours or so, with continuous stirring. After cooling to ambient temperature, the organic phase was separated from the aqueous phase. Gas chromatography and mass spectrometry (GC and GCMS) revealed a product containing 85% 3-octanoylthio-1-propyltriethoxysilane and 5.5% residual 3-chloro-1-propyltriethoxysilane (reported purities are based on area percent GC responses). Vacuum stripping at 110° C. at 0.1 torr to remove volatiles, primarily 3-chloro-1-propyltriethoxysilane, yielded a product of 90+% purity. Product identity using this process confirmed by nuclear magnetic resonance spectroscopy (NMR).

1. additionTo this solution was added
2. temperatureThis temperature was then maintained for 5-6 hours, with continued stirring
3. customwas then ramped up to 70° C. over the next 7 minutes
4. temperaturemaintained for about another 2 hours, with continued stirring, whereupon the temperature
5. temperaturewas raised to and
6. temperaturesubsequently maintained at 78° C. for an additional 24 hours
7. temperatureAfter cooling to ambient temperature
8. customthe organic phase was separated from the aqueous phase
9. additioncontaining 85% 3-octanoylthio-1-propyltriethoxysilane and 5.5% residual 3-chloro-1-propyltriethoxysilane (reported purities are based on area percent GC responses)
10. customstripping at 110° C. at 0.1 torr
11. customto remove volatiles, primarily 3-chloro-1-propyltriethoxysilane
12. customyielded a product of 90+% purity