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Methods for producing diorganodialkoxysilanes

Assignee: Lanxess Organometallics GmbH
•
Filing: 1989-06-26
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Granted: 1990-09-18
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Expires: 2009-06-26
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Abstract

Abstract In a method for the selective production of diorganodialkoxysilanes of the general formula ##STR1## by reaction of tetraalkoxysilanes of the formula Si(OR 3 ) 4 and monoorganotrialkoxysilanes of the formula R 1 Si(OR 3 ) 3 respectively with Grignard reagents, the desired reaction products are produced in high yield and without undesirable by-products and in high yield.

Inventors

  • 👤 Jurgen Graefe
  • 👤 Wolfram Uzick
  • 👤 Udo Weinberg

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 10:35
CPC Classifications
C; C07; C07F; C07F7/00; C07F7/02; C07F7/08; C07F7/0834; C07F7/0838; C07F7/0872; C07F7/0876; C07F7/0878; C07F7/18; C07F7/1804; C07F7/1872; C07F7/1876

Claims Analysis

Total Claims: 31
Claim 1
Independent Claim 151 words
A method of selective production of diorganodialkoxysilane having the general formula: ##STR11## which comprises reacting at a temperature of about 0° to about 90° C. a tetraalkoxysilane having the formula Si(OR 3 ) 4 or a monoorganotrialkoxysilanes having the formula R 1 Si(OR 3 ) 3 with an alkylating effective amount of a Grignard reagent having the formula R 2 MgX, wherein X is Br, Cl or I; R 1 and R 2 are independently an alkyl group or a cycloalkyl group having 3 to 10 carbon atoms, wherein at least one of R 1 and R 2 is a branched alkyl group having the branched alkyl group at the α- or β- carbon to the Si; R 1 is R 2 when reacting the tetraalkoxysilane with the Grignard reagent; and. each R 3 may be the same or different and is an alkyl group having 1 to 5 carbon atoms.
Claim 2
Independent Claim 151 words
A method of selective production of diorganodialkoxysilane having the general formula: ##STR11## which comprises reacting at a temperature of about 0° to about 90° C. a tetraalkoxysilane having the formula Si(OR 3 ) 4 or a monoorganotrialkoxysilanes having the formula R 1 Si(OR 3 ) 3 with an alkylating effective amount of a Grignard reagent having the formula R 2 MgX, wherein X is Br, Cl or I; R 1 and R 2 are independently an alkyl group or a cycloalkyl group having 3 to 10 carbon atoms, wherein at least one of R 1 and R 2 is a branched alkyl group having the branched alkyl group at the α- or β- carbon to the Si; R 1 is R 2 when reacting the tetraalkoxysilane with the Grignard reagent; and. each R 3 may be the same or different and is an alkyl group having 1 to 5 carbon atoms.
Claim 3
Dependent Claim 67 words
The method according to claim 1 wherein R 1 or R 2 is ##STR12## wherein y is 1 or 0; R 4 is alkyl having 1 to 7 carbon atoms; R 5 is alkyl having 1 to 7 carbon atoms; or R 4 and R 5 taken together with the carbon atom to which they are attached form a cycloalkyl group having 3 to 10 carbon atoms.
Claim 4
Dependent Claim 27 words
The method of selective production of dialkyldialkoxysilanes according to claim 1 wherein R 1 and R 2 are branched alkyl groups having 3 to 6 carbon atoms.
Claim 5
Dependent Claim 26 words
The method of selective production of dicycloalkyldialkoxysilanes according to claim 1, wherein R 1 and R 2 are cycloalkyl groups having 5 to 7 carbon atoms.
Claim 6
Dependent Claim 38 words
The method of selective production of alkylcycloalkyldialkoxysilanes according to claim 1, wherein R 1 is a branched alkyl group having 3 to 6 carbon atoms and R 2 is a cycloalkyl group having 5 to 7 carbon atoms.
Claim 7
Independent Claim 25 words
The method of selective production of diorganodialkoxysilanes according to any one of claims 1 to 5, wherein R 3 is a methyl or ethyl group.
Claim 8
Independent Claim 22 words
The method according to any one of claims 1 to 5, wherein the Grignard reagent (R 2 MgX) is formed in situ.
Claim 9
Independent Claim 17 words
The method according to any one of claims 1 to 5, wherein X is Cl or Br.
Claim 10
Dependent Claim 12 words
The method of claim 1, wherein the reaction is conducted in methyl-tert-butylether.
Claim 11
Dependent Claim 33 words
The method of claim 1 which comprises quenching any excess Grignard reagent remaining after reaction with a stoichiometric amount of an alcohol R 3 OH thereby forming a side product R 3 OMgX.
Claim 12
Dependent Claim 29 words
The method of claim 1 wherein the effective amount of the Grignard reagent is present in a molar ratio of tetraalkoxysilane to Grignard reagent ranging from 1:2 to 1:10.
Claim 13
Dependent Claim 15 words
The method of claim 11 wherein the molar ratio range is from 1:2 to 1:5.
Claim 14
Dependent Claim 29 words
The method of claim 1 wherein the effective amount of the Grignard reagent is present in a molar ratio of monoorganotrialkoxysilane to Grignard reagent ranging from 1:1 to 1:10.
Claim 15
Dependent Claim 14 words
The method of claim 13 wherein the molar ratio ranges from 1:1 to 1:3.
Claim 16
Dependent Claim 112 words
The method of claim 1 wherein the monoorganotrialkoxysilane is sec-butyltrimethoxysilane, the Grignard reagent is isobutylmagnesium chloride and the product is isobutyl-sec-butyldimethoxysilane; the monoorganotrialkoxysilane is isobutyltrmethoxysilane, the Grignard reagent is n-propylmagnesium chloride and the product is isobutyy-n-propyltrimethoxysilane; the monoorganotrialkoxysilane is isobutyltrimethoxysilane, the Grignard reagent is isopropylmagnesium chloride and the product is isobutylisopropyldimethoxysilane; the monoorganotrialkoxysilane is isobutyltrimethoxysilane, the Grignard reagent is cyclopentylmagnesium chloride and the product is isobutylcyclopentyldimethoxysilane; the monoorganotrialkoxysilane is isobutyltrimethoxysilane, the Grignard reagent is cyclohexylmagnesium chloride and the product is isobutylcyclohexyldimethoxysilane; the monoorganotrialkoxysilane is n-octyltriethoxysilane, the Grignard reagent is sec-butylmagnesium chloride and the product is n-octyl-secbutyldiethoxysilane or the monoorganotrialkoxysilane is isopropyltripropoxysilane, the Grignard reagent is cyclopentylmagnesium chloride and the product is isopropylcyclopentyldipropoxysilane.
Claim 17
Dependent Claim 82 words
The method of claim 1 wherein the tetraalkoxysilane is tetramethoxysilane, the Grignard reagent is isopropylmagnesium chloride and the product is diisopropyldimethoxysilane; the tetraalkoxysilane is tetramethoxysilane, the Grignard reagent is cyclopentylmagnesium chloride and the product is dicyclopentyldimethoxysilane; the tetraalkoxysilane is tetramethoxysilane, the Grignard reagent is isoamylmagnesium chloride and the product is diisoamyldimethoxysilane; the tetraalkoxysilane is tetrapropoxysilane, the Grignard reagent is sec-butylmagnesium chloride and the product is di-sec-butyldipropoxysilane or the tetraalkoxysilane is tetrapentoxysilane, the Grignard reagent is sec-butylmagnesium chloride and the product is di-sec-butyldipentoxysilane.
Claim 18
Dependent Claim 140 words
In a process for preparing a diorganodialkoxysilane having the formula ##STR13## by reacting a tetraalkoxysilane of the formula Si(OR 3 ) 4 with an alkylating agent, the improvement comprises selecting as the alkylating agent a Grignard reagent having a secondary carbon atom, of the formula R 2 MgX wherein R 2 is ##STR14## R 4 is alkyl having 1 to 7 carbon atoms, R 5 is alkyl having 1 to 7 carbon atoms, or R 4 and R 5 taken together form a cycloalkyl group having 3 to 10 carbon atoms, each R 3 is the same or different and is alkyl having 1 to 5 carbon atoms, and X is Cl, Br and I, and y=0 or 1, reacting an alkylating-effective amount of said Grignard reagent with said tetraalkoxysilane and thereby forming a substantially pure diorganodialkoxysilane in quantitative yields.
Claim 19
Dependent Claim 140 words
In a process for preparing a diorganodialkoxysilane having the formula ##STR13## by reacting a tetraalkoxysilane of the formula Si(OR 3 ) 4 with an alkylating agent, the improvement comprises selecting as the alkylating agent a Grignard reagent having a secondary carbon atom, of the formula R 2 MgX wherein R 2 is ##STR14## R 4 is alkyl having 1 to 7 carbon atoms, R 5 is alkyl having 1 to 7 carbon atoms, or R 4 and R 5 taken together form a cycloalkyl group having 3 to 10 carbon atoms, each R 3 is the same or different and is alkyl having 1 to 5 carbon atoms, and X is Cl, Br and I, and y=0 or 1, reacting an alkylating-effective amount of said Grignard reagent with said tetraalkoxysilane and thereby forming a substantially pure diorganodialkoxysilane in quantitative yields.
Claim 20
Dependent Claim 18 words
The improved process of claim 17 wherein the yield is greater than 95% and purity greater than 97%.
Claim 21
Dependent Claim 30 words
The improved process according to claim 17 wherein the effective amount of Grignard reagent is present in a molar ratio of tetraalkoxysilane to Grignard reagent ranging from 1:2 to 1:10.
Claim 22
Dependent Claim 16 words
The improved process according to claim 19 wherein the molar ratio range from 1:2 to 1:5.
Claim 23
Dependent Claim 13 words
The improved process of claim 17, wherein the reaction is conducted in methyl-tert-butylether.
Claim 24
Dependent Claim 34 words
The improved process of claim 17 which comprises quenching any excess Grignard reagent remaining after reaction with a stoichiometric amount of an alcohol R 3 OH thereby forming a side product R 3 OMgX.
Claim 25
Dependent Claim 194 words
In a process for preparing a diorganodialkoxysilane having the formula ##STR15## by reacting an alkylating agent with a monoorganotrialkoxysilane, the improvement which comprises selecting a monoorganotrialkoxysilane having a secondary carbon atom or an alkylating agent having a secondary carbon atom, wherein the monoorganotrialkoxysilane has the formula R 1 Si(OR 3 ) 3 and the Grignard reagent has the formula R 2 MgX, and one of R 1 and R 2 is ##STR16## and the other is n-alkyl having 3 to 10 carbon atoms or is ##STR17## R 4 is alkyl having 1 to 7 carbon atoms, R 5 is alkyl having 1 to 7 carbon atoms, or R 4 and R 5 taken together with the carbon atom to which they are attached form a cycloalkyl group having 3 to 10 carbon atoms, each R 3 may be the same or different and is alkyl having 1 to 5 carbon atoms, X is Br, Cl or I, and y is 0 or 1, reacting at a temperature of about 0° to about 90° C. an alkylating-effective amount of said Grignard reagent with said monoorganotrialkoxysilane and thereby forming a substantially pure diorganodialkoxysilane in quantitative yields.
Claim 26
Dependent Claim 194 words
In a process for preparing a diorganodialkoxysilane having the formula ##STR15## by reacting an alkylating agent with a monoorganotrialkoxysilane, the improvement which comprises selecting a monoorganotrialkoxysilane having a secondary carbon atom or an alkylating agent having a secondary carbon atom, wherein the monoorganotrialkoxysilane has the formula R 1 Si(OR 3 ) 3 and the Grignard reagent has the formula R 2 MgX, and one of R 1 and R 2 is ##STR16## and the other is n-alkyl having 3 to 10 carbon atoms or is ##STR17## R 4 is alkyl having 1 to 7 carbon atoms, R 5 is alkyl having 1 to 7 carbon atoms, or R 4 and R 5 taken together with the carbon atom to which they are attached form a cycloalkyl group having 3 to 10 carbon atoms, each R 3 may be the same or different and is alkyl having 1 to 5 carbon atoms, X is Br, Cl or I, and y is 0 or 1, reacting at a temperature of about 0° to about 90° C. an alkylating-effective amount of said Grignard reagent with said monoorganotrialkoxysilane and thereby forming a substantially pure diorganodialkoxysilane in quantitative yields.
Claim 27
Dependent Claim 18 words
The improved process of claim 23 wherein the yield is greater than 95% and purity greater than 97%.
Claim 28
Dependent Claim 30 words
The improved process according to claim 23 wherein the effective amount of Grignard reagent is present in a molar ratio of monoorganotrialkoxysilane to Grignard reagent ranging from 1:1 to 1:10.
Claim 29
Dependent Claim 16 words
The improved process according to claim 25 wherein the molar ratio ranges from 1:1 to 1:3.
Claim 30
Dependent Claim 13 words
The improved process of claim 23, wherein the reaction is conducted in methyl-tert-butylether.
Claim 31
Dependent Claim 34 words
The improved process of claim 23 which comprises quenching any excess Grignard reagent remaining after reaction with a stoichiometric amount of an alcohol R 3 OH thereby forming a side product R 3 OMgX.

References Cited (Backward Citations)

US2380057A Cited
US2414505A Cited
US2671101A Cited
US2671795A Cited
US2709692A Cited
US4748262A Cited
US4777278A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1993-09-17 1994-03-19 1994-09-18 $2000.00 Window Closed / Lapsed
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