関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexachlorodisilane | HCID 83497 | — |
| 反応物 | Lithium N-methylmethanaminide | HCID 5152226 | — |
| 反応物 | (2S,3S)-2-[4-[(1R)-1-amino-2-hydroxyethyl]triazol-1-yl]-1-[4-[4-[4-[(2S,3S)-2-[4-[(1R)-1-amino-2-hydroxyethyl]triazol-1-yl]-3-methylpentanoyl]piperazin-1-yl]-6-[2-[2-(2-prop-2-ynoxyethoxy)ethoxy]ethylamino]-1,3,5-triazin-2-yl]piperazin-1-yl]-3-methylpentan-1-one;hydrochloride | HCID 16745346 | — |
| 反応物 | Pentakis(dimethylamino) chloro disilane | HCID 86638304 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Hexakis(dimethylamino) disilane | HCID 22053281 | — |
反応手順
The synthesis of ClSi2(NMe2)5 has been done from the ammonolysis of hexachlorodisilane and lithium dimethylamide. Hexachlorodisilane (HCD) is used as the starting material so that the Si—Si direct bond remains in the molecule. n-hexane is used as a solvent and cooled at 0° C. A mixture of pentakis(dimethylamino) chloro disilane and hexakis(dimethylamino) disilane is obtained. Lithium dimethylamide is added to form a “lithium dimethylamide solution”. HCD is added dropwise in the 0° C. lithium dimethylamide solution. Then the solution is stirred for 2 h at 0° C. then for 15 h at RT. The salt LiCl is then removed from the solution, and the n-hexane removed in vacuo. The resulting ClSi2(NMe2)5 and other byproducts are separated by fractional distillation. The NMR spectra indicates that the samples obtained from this distillation process contain less than 5% vol of Si2(NMe2)6.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08377511B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-3de5682d66d94f2b8b4f54e227e81f6c |
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| 出典メモ | uspto-grants-2013_02 |
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