Hexachlorodisilane → Hexakis(dimethylamino) disilane

HRID 388181

Reaktionsgleichung

Reaktionsgleichung von HRID 388181
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]

Komponenten

6

Edukt 4

HCID 83497Hexachlorodisilane2×HCID 5152226Lithium N-methylmethanaminideHCID 16745346(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;hydrochlorideHCID 86638304Pentakis(dimethylamino) chloro disilane

Produkt 1

HCID 22053281Hexakis(dimethylamino) disilane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8058HexaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

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.

Quellen und Nachweise

ORD-Eintrag
ord-3de5682d66d94f2b8b4f54e227e81f6c
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08377511B2

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