Hexachlorodisilane → Hexakis(dimethylamino) disilane

HRID 1692151

Reaction equation

HRID 1692151 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.

Sources & evidence

ORD record
ord-00e69f087e304ee28f73864974a68a5b
Source dataset
uspto-grants-2012_04
Patent number
US08153832B2

Linked notes

Loading…