Aminoiodosilanes and methods of synthesizing these aminoiodosilanes

• US 10,640,523 B2
• Filed: 01/08/2019
• Issued: 05/05/2020
• Est. Priority Date: 01/12/2018
• Status: Active Grant

• Current Assignee: Entegris Incorporated
• Original Assignee: Entegris Incorporated
• Inventors: Baum, Thomas H., Khandelwal, Manish, Kuiper, David
• Primary Examiner(s): Brooks, Clinton A
• Assistant Examiner(s): Adzamli, Kofi
• Application Number:
  US16/242,706
• Publication Number:
  US 20190218238A1
• Time in Patent Office: 483 Days
• Field of Search: None
• CPC Class Codes: B01D 3/10 Vacuum distillation B01D3/12 takes precedence
• CPC Class Codes: C07F 13/005 Compounds without a metal-carbon linkage
• CPC Class Codes: C07F 7/10 containing nitrogen having a Si-N linkage

Abstract

Methods of synthesizing aminoiodosilanes are disclosed. The reaction to produce the disclosed aminoiodosilanes is represented by the formula:
SiI₄+z(NH₂R¹)=SiI_y(NHR¹)_z,
wherein R¹ is selected from a C₁-C₁₀ alkyl or cycloalkyl, aryl, or a hetero group; y=1 to 3; and z=4−y.

Claims

1. A method of synthesizing an aminoiodosilane comprising:

contacting an iodosilane having the formula SiI₄ with an monosubstituted amine having the formula NH₂R¹ to produce an aminoiodosilane reaction product having the formula SiI_y(NHR¹)_z, wherein R¹ is selected from a C₁-C₁₀ alkyl or cycloalkyl, aryl, or a hetero group;

y=1 to 3; and

z=4−

y.

2. The method of claim 1, wherein a molar ratio of the iodosilane to the monosubstituted amine ranges from approximately 1:

2 to 1;

4.

3. The method of claim 1, further comprising isolating the aminoiodosilane reaction product from a crude mixture produced by the reaction.

4. The method of claim 1, further comprising vacuum distilling the aminoiodosilane reaction product.

5. The method of claim 1, wherein the method produces an aminoiodosilane reaction product and an alkylammoniuim iodide salt.

6. The method of claim 1, wherein the reaction is performed in a solvent.

7. The method of claim 6, wherein the solvent is toluene.

8. The method of claim 1, wherein the monosubstituted amine is t-butylamine and the aminoiodosilane is t-butylaminotriiodosilane.

9. The method of claim 1, wherein the monosubstituted amine is methylamine or ethylamine and the aminoiodosilane is methylaminotriiodosilane or ethylaminotriiodosilane.

10. The method of claim 1, wherein the monosubstituted amine is isopropylamine and the aminoiodosilane is isopropylaminotriiodosilane.

11. The method of claim 1, wherein the aminoiodosilane is bis(t-butylamino)diiodosilane or bis(isopropylamino)diiodosilane.

12. The method of claim 1, wherein the amine is added to the iodosilane.