- Method for manufacturing of alkylaminosilane compound
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The present invention relates to a method for preparing alkylaminosilane compounds capable of obtaining high purity alkylaminosilane compounds in high yield.
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Paragraph 0083-0085
(2021/04/29)
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- METHOD FOR PRODUCING DIALKYLAMINOSILANE
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A method for safely and efficiently producing high-purity dialkylaminosilane. Dialkylamine is fed simultaneously during feeding chlorosilane in the presence of metal to cause reaction. For example, chlorosilane and dialkylamine are fed, and then only dialkylamine is fed to cause reaction, whereby dialkylaminosilane is produced.
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Paragraph 0051-0065; 0071-0089
(2020/05/06)
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- Synthetic method for tris(dimethylamino)silane
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A synthetic method for tris(dimethylamino)silane is disclosed. The method includes 1) preparing a reaction vessel and feeding protective gas; 2) cooling the reaction vessel to a temperature between -65 DEG C and -75 DEG C, adding a hydrocarbon solvent into the reaction vessel, then adding an organic lithium metal compound and stirring the mixture at a maintained low temperature; 3) feeding dimethylamine gas into the reaction vessel, and stirring the mixture at a maintained low temperature for 8-10 h to prepare a lithium salt of dimethylamine; and 4) while maintaining the low temperature between -65 DEG C and -75 DEG C, adding trichlorosilane to the reaction vessel, after the addition is finished, allowing the mixture to stand to allow the temperature to slowly rise to room temperature, andstirring the mixture for 8-10 h until the reaction is finished; and 5) performing atmospheric-vacuum distillation after the reaction is finished, and collecting a fraction of 75-80 DEG C/5-10 mmHg toobtain the tris(dimethylamino)silane. The cost and reaction toxicity are reduced, operation is simple, and the target compound can be directly obtained without the need of filtration, is high in purity, and meets high requirements of electronic chemicals on product quality.
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Paragraph 0019-0021
(2019/07/16)
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- 1,1,1-TRIS(ORGANOAMINO)DISILANE COMPOUNDS AND METHOD OF PREPARING SAME
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A 1,1,1-tris(organoamino)disilane compound and a method of preparing the 1,1,1-tris(organoamino)disilane compound are disclosed. The method comprises aminating a 1,1,1-trihalodisilane with an aminating agent comprising an organoamine compound to give a reaction product comprising the 1,1,1-tris(organoamino)disilane compound, thereby preparing the 1,1,1-tris(organoamino)disilane compound. A film-forming composition is also disclosed. The film-forming composition comprises the 1,1,1-tris(organoamino)disilane compound. A film formed with the film-forming composition, and a method of forming the film, are also disclosed. The method of forming the film comprises subjecting the film-forming composition comprising the 1,1,1-tris(organoamino)disilane compound to a deposition condition in the presence of a substrate, thereby forming the film on the substrate.
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Paragraph 0096-0097
(2019/02/15)
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- METHOD FOR PRODUCING DIALKYLAMINOSILANE
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In a method for synthesizing dialkylaminosilane from a reaction of dialkylamine with chlorosilane as the method for producing dialkylaminosilane, a large amount of dialkylamine hydrochloride is produced as a by-product, in addition to objective dialkylaminosilane. Therefore, upon obtaining objective dialkylaminosilane, reduction of volumetric efficiency caused by a large amount of a solvent is prevented, and dialkylaminosilane is produced at a low cost and in a large amount. Dialkylaminosilane having a small halogen content is produced with high volumetric efficiency by using, as a solvent upon allowing dialkylamine to react with chlorosilane, an aprotic polar solvent having high solubility in dialkylamine hydrochloride and metal chloride each produced as a by-product by the reaction, and straight-chain or branched hydrocarbon having high solubility in dialkylaminosilane and hard to dissolve a halogen compound therein.
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Paragraph 0053-0056
(2018/03/09)
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- PROCESS FOR THE PREPARATION OF TRISALKYLAMINOSILANE
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The present invention relates to a method of preparing tris(alkylamino)silane comprising the steps in which: (a) an amine represented by chemical formula of R^1R^2NH is made to react with a halosilane represented by chemical formula of SiH_nX_4-n; and (b) tris(alkylamino)silane, a product of the step (a), is made to react with a metal hydride and converted into tris(alkylamino)silane. In the chemical formulas, R^1 and R^2 each independently represent a linear, branched or cyclic alkyl group having 1 to 6 carbon atoms; n is 0 or 1; X is a fluoro-, chloro-, bromo-, or iodo-group; and the step (a) necessarily includes a compound in which n equals zero. According to the present invention, by using a metal hydride to reduce a tris(alkylamino)silane intermediate, which is a reaction product of amine and halosilane, and thus convert the same into tris(alkylamino)silane, tris(alkylamino)silane can be obtained in a high yield and alkylamine hydrochloride produced as a byproduct can be easily removed, and accordingly, the impurity content in the final product can be reduced to a few ppb or less.COPYRIGHT KIPO 2017
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Paragraph 0071; 0076-0077
(2017/08/02)
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- Method for removing compounds having Si-O bond from aminosilanes
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The present invention relates to a method for eliminating compounds having an Si-O bond from aminosilane. More specifically, the present invention relates to a method for eliminating compounds having an Si-O bond from aminosilane, which comprises the following steps: treating aminosilane including the compounds having Si-O bond as impurities with alkyl metal so as to transform the impurities into a compound showing large difference in the boiling point from aminosilane; and eliminating the impurities through distillation, thereby simplifying a distillation process and increasing yield of aminosilane.
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Paragraph 0021-0022
(2017/06/02)
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- METHOD FOR PREPARING PURIFIED AMINOSILANE
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An object is to provide a highly pure aminosilane having a reduced amount of halogen impurity, which is suitable for applications of electronic materials and others. More specifically, provided is a method for preparing a purified aminosilane comprising at least the steps of treating, with an alkyl metal reagent, an aminosilane having a Si—N bond but not a Si-halogen bond and having halogen impurity content of 1 ppm (w/w) or more; and distilling the treated aminosilane.
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Page/Page column 4
(2012/07/13)
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- Hydride and fluoride transfer reactions accompanying nucleophilic substitution at pentacoordinate silicon
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The syntheses of aminoazasilatranes of the type R2NSi(R′NCH2CH2)3N (R′ = H, R = H (2a), CH3 (3a), CH2CH3 (4a), Si(CH3)3 (6a), R′ = CH3, R = H (2b), CH3 (3b), CH2CH3 (4b), Si(CH3)3 (6b) via nucleophilic substitution reactions of ClSi(R′NCH2CH2)3N (R′ = H (7a), R′ = CH3 (7b), respectively) with amide anions are reported. Reactivities of 7a and 7b toward other nucleophilic reagents such as alkyllithiums and Group 1 metal alkoxides are also described. It is found that the equatorial NR′ functionalities significantly influence the reaction pathways. With strong bases, lithiation of the equatorial NH hydrogens of 7a predominated along with some nucleophilic substitution products and hydride transfer product HSi(HNCH2CH2)3N, 1a. With 7b, however, equatorial nitrogen lithiation is precluded and its reaction with nucleophiles can produce substantial amounts of nucleophilic substitution product as well as hydride transfer product HSi(CH3NCH2CH2)3N, 1b. The relative ratios of these products depend substantially on stereoelectronic factors, the nature of the nucleophilic reagents, and the reaction conditions. In the case of the reaction of 7b with BrC6F5/n-BuLi, three products, namely, C6F5Si(CH3NCH2CH2) 3N (13b), FSi(CH3NCH2CH2)3N (14b), and C6F5Si(CH3NCH2CH2) 2(ο-C6F4CH3NCH 2CH2)N (15) formed in an approximate ratio of 1:2:1. The formation of 15 is attributed to perfluorobenzyne insertion into a Si-Neq bond of (13b). Interestingly, the plane defined by the axial NSi2 moiety in 6a is found to be fixed at the apical position of the silicon, providing an interesting example of pπ-dπ interaction between a pentacoordinate silicon and a nitrogen. However, the axial moiety in analogue 6b freely rotates around the apical Si-N bond due to steric interactions with nearby methyl groups on the cage.
- Wan, Yanjian,Verkade, John G.
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p. 141 - 156
(2007/10/02)
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