Hexachlorodisilane → Hexakis(dimethylamino) disilane

HRID 388181

反応式

HRID 388181 の反応式
Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl.[CH3:9][N-:10][CH3:11].[Li+].CC[C@@H]([C@H](N1N=NC([C@@H](N)CO)=C1)C(N1CCN(C2N=C(NCCOCCOCCOCC#C)N=C(N3CCN(C([C@@H](N4N=NC([C@@H](N)CO)=C4)[C@H](CC)C)=O)CC3)N=2)CC1)=O)C.Cl.[CH3:77][N:78]([Si:80]([N:92]([CH3:94])[CH3:93])([N:89]([CH3:91])[CH3:90])[Si:81]([N:86]([CH3:88])[CH3:87])([N:83]([CH3:85])[CH3:84])Cl)[CH3:79]>CCCCCC>[CH3:9][N:10]([Si:81]([N:86]([CH3:88])[CH3:87])([N:83]([CH3:85])[CH3:84])[Si:80]([N:89]([CH3:91])[CH3:90])([N:92]([CH3:93])[CH3:94])[N:78]([CH3:77])[CH3:79])[CH3:11]

参加物

6

反応条件

温度
0 °C

実験手順

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.

出典と根拠

ORDレコード
ord-3de5682d66d94f2b8b4f54e227e81f6c
出典データセット
uspto-grants-2013_02
特許番号
US08377511B2

関連ノート

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