Hexachlorodisilane → Hexakis(dimethylamino) disilane

Participants

Role	Name	HCID	Charge
Reactant	Hexachlorodisilane	HCID 83497	—
Reactant	Lithium N-methylmethanaminide	HCID 5152226	—
Reactant	(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	—
Reactant	Pentakis(dimethylamino) chloro disilane	HCID 86638304	—
Solvent	Hexane	HCID 8058	—
Product	Hexakis(dimethylamino) disilane	HCID 22053281	—

Reaction Conditions

Temperature	0 °C

Reaction Steps

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.

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US08377511B2
Source dataset	uspto-grants-2013_02
ORD ID	ord-3de5682d66d94f2b8b4f54e227e81f6c
Source note	uspto-grants-2013_02