Method of preparing pentachlorodisilane purified reaction product comprising same
A method of preparing pentachlorodisilane is disclosed. The method comprises partially reducing hexachlorodisilane with a metal hydride compound to give a reaction product comprising pentachlorodisilane. The method further comprises purifying the reaction product to give a purified reaction product comprising the pentachlorodisilane. The purified reaction product comprising pentachlorodisilane formed in accordance with the method is also disclosed.
1. A method of preparing pentachlorodisilane, said method comprising:
partially reducing hexachlorodisilane with a metal hydride compound to give a reaction product comprising pentachlorodisilane; and
purifying the reaction product to give a purified reaction product comprising pentachlorodisilane, wherein purifying the reaction product comprises:
distilling the reaction product to prepare a plurality of crude reaction products comprising pentachlorodisilane;
combining the plurality of crude reaction products to give a combined crude reaction product; and
fractionally purifying the combined crude reaction product to give the purified reaction product.
2. The method of claim 1 , wherein the metal hydride compound comprises diisobutylaluminum hydride (DIBAH).
3. The method of claim 1 , wherein the purified reaction product comprises pentachlorodisilane in an amount of at least 95 wt. % based on the total weight of the purified reaction product.
4. The method of claim 3 , wherein the purified reaction product comprises pentachlorodisilane in an amount of at least 98 wt. % based on the total weight of the purified reaction product.
5. The method of claim 1 , wherein distilling the reaction product is carried out at a reduced pressure and an elevated temperature.
6. The method of claim 5 , wherein: (i) the reduced pressure is from greater than 0 to 50 Torr; (ii) the elevated temperature is from 70 to 90° C.; or (iii) both (i) and (ii).
7. The method of claim 1 , wherein: (i) the hexachlorodisilane and metal hydride compound are utilized in a molar ratio of from 1:0.01 to 1:3; (ii) the method is carried out in the absence of any solvent; (iii) partially reducing the hexachlorodisilane is carried out at an elevated temperature; (iv) purifying the reaction product comprises a plurality of purification steps; or (v) any combination of (i) to (iv).