Process of synthesizing diisopropylamino-disilanes

Patent metadata

Field	Value
Publication number	US-9840523-B2
Application number	US-201515300987-A
Country	US
Kind code	B2
Filing date	May 29, 2015
Priority date	May 30, 2014
Publication date	Dec 12, 2017
Grant date	Dec 12, 2017

Abstract

Chemical processes comprise selectively synthesizing diisopropylamino-disilanes and reduction of chloride in aminosilanes, and the compositions comprise the diisopropylamino-disilanes and at least one reaction by-product prepared thereby. The diisopropylamino-disilanes are diisopropylamino-pentachlorodisilane and diisopropylamino-disilane.

First claim

What is claimed is:

1. A process of synthesizing diisopropylamino-disilane, which is of formula (I): [(CH 3 ) 2 CH] 2 NSiH 2 SiH 3 (I), the process comprising:
contacting in a solvent, a metal aluminum hydride with diisopropylamino-pentachlorodisilane, to give diisopropylamino-disilane, wherein the metal of the metal aluminum hydride is an element of Group I or Group II of the Periodic Table of the Elements; and
separating the diisopropylamino-disilane from the solvent and an optional second solvent to give a purified form of the diisopropylamino-disilane, wherein the solvent or the optional second solvent has a boiling point of at least 90° C. and at least 10° C. higher than the boiling point of diisopropylamino-disilane, and wherein the optional second solvent is combined with the solvent before, after, or during the contacting and prior to the separating.

2. The process of claim 1 comprising one of the following limitations e) or f):
e) wherein the solvent or the optional second solvent is an alkylene glycol dialkyl ether and the alkylene glycol dialkyl ether is a tetraethylene glycol di(C 1 -C 4 )alkyl ether, propylene glycol di(C 4 -C 8 )alkyl ether, ethylene glycol di(C 4 or C 8 )alkyl ether, or a combination of any two or more thereof
f) wherein the solvent is characterizable by a boiling point that is at least 10° C. less than the boiling point of the diisopropylamino-disilane; the second solvent is present and is characterizable by a boiling point that is at least 10° C. higher than the boiling point of the diisopropylamino-disilane; the solvent is first separated from the diisopropylamino-disilane and the second solvent and then the diisopropylamino-disilane is separated from the second solvent to give a purified form of the diisopropylamino-disilane in at least 30% yield and purity of at least 70 area % (GC).

3. A process of synthesizing diisopropylamino-disilane, which is of formula (I):
[(CH 3 ) 2 CH] 2 NSiH 2 SiH 3   (I), the process comprising parts A and B:

Part A:

contacting, in a hydrocarbon vehicle, hexachlorodisilane (SiCl 3 SiCl 3 ) with, relative to the hexachlorodisilane, from 0.50 to 1.19 molar equivalents of a metal diisopropylamide, [(i-Pr) 2 N] m M A , wherein subscript m is 1 or 2, wherein when m is 1, M A is an element of Group I of the Periodic Table of the Elements and when m is 2, M A is an element of Group II of the Periodic Table of the Elements, or with from 1.0 to 2.39 molar equivalents of diisopropylamine, or with a mixture of from 0.50 to 1.19 molar equivalents of diisopropylamine ((i-Pr) 2 NH) and from 0.50 to 1.19 molar equivalents of triethylamine (Et 3 N), to give a higher yield of diisopropylamino-pentachlorodisilane compared to the yield, if any, of a compound of formula (B): [(CH 3 ) 2 CH] 2 NSiCl 2 SiCl 2 N[CH(CH 3 ) 2 ] 2 (B), wherein i-Pr is isopropyl and Et is ethyl; and
Part B:

Contacting, in an alkylene glycol dialkyl ether characterizable by a boiling point, lithium aluminum hydride (LiAlH 4 ) with the diisopropylamino-pentachlorodisilane from Part A to give diisopropylamino-disilane characterizable by a boiling point, wherein the boiling point of the alkylene glycol dialkyl ether is at least 30 degrees Celsius higher than the boiling point of diisopropylamino-disilane; and
Separating the diisopropylamino-disilane from the alkylene glycol dialkyl ether to give a purified form of the diisopropylamino-disilane in at least 30% yield for Part B and a purity greater than or equal to 70 area % (GC).

4. The process of claim 1 further comprising combining i) a metal hydride or ii) a metal amide salt with the diisopropylaminodisilane either before or after the separating.

5. The process of claim 4 , wherein the metal hydride is lithium tris-(tert-butoxy)-aluminum hydride, lithium triethylborohydride, or sodium triethylborohydride and the metal amide is lithium diisopropylamide.

6. A process of synthesizing diisopropylamino-disilane according to claim 1 , wherein the contacting is under vacuum and at a temperature to vaporize the diisopropylamino-disilane after it is formed; and
separating the diisopropylamino-disilane after it is formed from unreacted diisopropylamino-pentachlorodisilane and the metal aluminum hydride by distillation, wherein the distillation is conducted concurrently with the formation of the diisopropylamino-disilane.

7. The process of claim 6 , wherein the contacting is at a temperature of at least 90° C.

Assignees

• Dow Corning

Inventors

• Ketola Barry M
• Rekken Brian D
• Zhou Xiaobing

Classifications

• C07F7/126

  by reactions involving the formation of Si-Y linkages, where Y is not a carbon or halogen atom · CPC title

• C07F7/10 Primary

  containing nitrogen {having a Si-N linkage} · CPC title

• C07F7/081

  comprising at least one atom selected from the elements N, O, halogen, S, Se or Te · CPC title

• C07F7/12

  Organo silicon halides · CPC title

• C07F7/20

  Purification, separation · CPC title