Synthesis of SiCl4 via the Chloride Salt-Catalyzed Reaction of Orthosilicates with SOCl2
This paper details a method to chlorinate tetraalkyl orthosilicates in the presence of a catalyst using SOCl2 as the chloride source/deoxygenating agent. Several inexpensive catalysts were screened, and it was found that soluble chloride salts performed better than Lewis base catalysts. The optimize...
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| Published in | Industrial & engineering chemistry research Vol. 56; no. 40; pp. 11652 - 11655 |
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| Main Authors | , , , |
| Format | Journal Article |
| Language | English |
| Published |
American Chemical Society
11.10.2017
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| Subjects | |
| Online Access | Get full text |
| ISSN | 0888-5885 1520-5045 1520-5045 |
| DOI | 10.1021/acs.iecr.7b03301 |
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| Abstract | This paper details a method to chlorinate tetraalkyl orthosilicates in the presence of a catalyst using SOCl2 as the chloride source/deoxygenating agent. Several inexpensive catalysts were screened, and it was found that soluble chloride salts performed better than Lewis base catalysts. The optimized reaction employed a widely used and commercially available soluble chloride salt catalyst (e.g., NBu4Cl, 0.4 equiv), 16 equiv of SOCl2, and afforded quantitative yield of SiCl4 after 3 h. As the bulk of the orthosilicate substrate increased, the yield of SiCl4 decreased. A reaction mechanism has been proposed. |
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| AbstractList | This paper details a method to chlorinate tetraalkyl orthosilicates in the presence of a catalyst using SOCl₂ as the chloride source/deoxygenating agent. Several inexpensive catalysts were screened, and it was found that soluble chloride salts performed better than Lewis base catalysts. The optimized reaction employed a widely used and commercially available soluble chloride salt catalyst (e.g., NBu₄Cl, 0.4 equiv), 16 equiv of SOCl₂, and afforded quantitative yield of SiCl₄ after 3 h. As the bulk of the orthosilicate substrate increased, the yield of SiCl₄ decreased. A reaction mechanism has been proposed. This paper details a method to chlorinate tetraalkyl orthosilicates in the presence of a catalyst using SOCl2 as the chloride source/deoxygenating agent. Several inexpensive catalysts were screened, and it was found that soluble chloride salts performed better than Lewis base catalysts. The optimized reaction employed a widely used and commercially available soluble chloride salt catalyst (e.g., NBu4Cl, 0.4 equiv), 16 equiv of SOCl2, and afforded quantitative yield of SiCl4 after 3 h. As the bulk of the orthosilicate substrate increased, the yield of SiCl4 decreased. A reaction mechanism has been proposed. |
| Author | Placke, Jessica L Roberts, John M Katsoulis, Dimitris E Eldred, Donald V |
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| Snippet | This paper details a method to chlorinate tetraalkyl orthosilicates in the presence of a catalyst using SOCl2 as the chloride source/deoxygenating agent.... This paper details a method to chlorinate tetraalkyl orthosilicates in the presence of a catalyst using SOCl₂ as the chloride source/deoxygenating agent.... |
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| Title | Synthesis of SiCl4 via the Chloride Salt-Catalyzed Reaction of Orthosilicates with SOCl2 |
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