Hexachlorodisilane → Hexakis(dimethylamino) disilane

HRID 388181

Reaction equation

HRID 388181 reaction equation
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]

Participants

6

Reactant 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

Product 1

HCID 22053281Hexakis(dimethylamino) disilane

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Conditions

Temperature
0 °C

Procedure

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.

Sources & evidence

ORD record
ord-3de5682d66d94f2b8b4f54e227e81f6c
Source dataset
uspto-grants-2013_02
Patent number
US08377511B2

Linked notes

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