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ChemicalBook CAS DataBase List 3-Mercaptopropyltriethoxysilane
14814-09-6

3-Mercaptopropyltriethoxysilane synthesis

12synthesis methods
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Yield:14814-09-6 74% ,64-17-5 1.06 %Chromat.

Reaction Conditions:

with sodium hydrogensulfide;hydrogen sulfide;N-[bis(diethylamino)methylene]-N-ethylethane ammonium chloride in water at 98; under 879.175 - 1034.32 Torr; for 6 h;Product distribution / selectivity;

Steps:

1
Example 1; The reaction apparatus included a 1000 mL 45 psig-rated pressure glassware with “Hi-Pressure” Teflon fittings, mechanical stirrer, temperature control, heating mantle, and a source of H2S gas (lecture bottles from Sigma-Aldrich, Milwaukee, Wis.).The reactor was charged with 198 grams 45% aqueous NaSH solution (89.1 grams pure NaSH, 1.59 mmoles) and 114.1 grams 35% hexaethylguanidinium chloride (HEGCl) aqueous solution (40 grams pure, 0.15 mmoles), under stirring. Also, 360.4 grams (1.5 mmoles) of chloropropyltriethoxysilane (CPTES) were batch charged to the reactor. From a lecture bottle, H2S pressure was generated in the reactor to about 17 psi. The system was heated to 98° C., while the pressure increased to about 20 psi and maintained under these condition for about 6 hours. After cooling to room temperature, the H2S was vented off and an additional 275 grams of water were charged to the reactor. After stopping the agitation and phase separation, the top layer (346.2 grams) was removed and analyzed by gas chromatography (GC), revealing the following composition: 1.06 weight % ethanol, 19.9 weight % unreacted CPTES, 73.4 weight % mercaptopropyltriethoxysilane (MPTES), and 4.8 weight % heavies. The molar yield of MPTES was 74% based on CPTES.

References:

General Electric Company US7151188, 2006, B1 Location in patent:Page/Page column 4-5

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