Organosilicon Heteropolymers and Heterocompounds

Lukevit︠s︡, Ė. I︠A︡ (Ėdmund I︠A︡novich)
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Tetramethyldisiloxane TMDS , Boron trifluoride diethyl etherate BF3-OEt 2 , Dry ice was placed in the first dry ice condenser. The BF3- OEt 2 was added drop-wise to the reaction flask over a 25 minute period. After no more volatile material was coming over, the collected material was transferred to an evacuated stainless steel cylinder.

The collected product was 83 wt.

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Rubber septa were secured on the remaining two necks. Allyl cyanide 9. Karstedt's catalyst 0. A total of This reaction product was combined with the product from the following paragraph for purification by distillation. In a similar manner as described above, allyl cyanide 6. A total of 8.

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Abele, M. Request Username Can't sign in? Mixtures of such cyclic siloxanes may be employed as a starting material. Popelis, L. Boron trifluoride diethyl etherate BF3-OEt 2 , The resulting alkoxide solution can be ammoniated to produce the corresponding hydroxy aluminosilicate which can be dried in vacuum to produce mullite powders. Complex Salts of Iron with Organosilicon Compounds -- 5.

The reaction mixture was combined with the material described in the previous paragraph and the combined mixture was purified by distillation. After first removing a fore-cut containing toluene, water and other impurities, the desired product FIS3MN was isolated under full vacuum 0. Total product recovered was Bis 3-cyanopropyl tetramethyldisiloxane Boron trifluoride diethyl etherate BF3-OEt 2 Dry ice was placed in the dry ice condenser.

After the specified time, the reaction mixture was cooled and transferred to a separatory funnel. The layers were separated and the aqueous layer was washed with additional toluene approx.. The organic layers were combined into a ml round bottom flask which was connected to a short path distillation head with water cooled condenser. The total product collected was A portion of the product was analyzed by Karl Fisher technique and determined to contain just 62 ppm H2O by weight.

An apparatus and procedure as described in Example 1 was used for Example 4. Thus, 2,4,6, 8-tetramethylcyclotetrasiloxane Boron trifluoride diethyl etherate BF3- OEt 2 BF3 - OEt 2 was added drop- wise to the reaction flask over 25 minutes. No reflux or significant exotherm was observed. The volatile product was collected in the second two neck flask and subsequently transferred to a storage cylinder.

The collected product Thus, a fresh sample of allyl cyanide, The heating was shut off and the reaction mixture allowed to cool overnight. Analysis of the reaction mixture indicated complete conversion of allyl cyanide. The product was isolated under full vacuum 0. Total product recovered by distillation was The product also contained 0.

Dichloromethylsilane, DCMS, The product was collected at reduced pressure 0. The product identification was confirmed by tfNMR. The fluorination reaction may be carried out by contacting the DCS2MN with ammonium bifluoride for a time and at a temperature effective to replace the chlorine atoms present in the DCS2MN with fluorine atoms. In some cases, it is advantageous to carry out this reaction in an inert solvent capable of forming an azeotrope with water, such as an aromatic hydrocarbon e. Ref document number : Country of ref document : EP.

Organosilicon Heteropolymers and Heterocompounds - S N Borisov - Häftad () | Bokus

Kind code of ref document : A1. Country of ref document : US. Ref country code : DE. Methods of synthesizing fluorosilanes containing cyano-substituted alkyl groups are provided. For example, 3-cyanopropyldimethylfluorosilane may be produced by reacting tetramethyldisiloxane and boron trifluoride to obtain fluorodimethylsilane and then reacting the fluorodimethylsilane with allyl cyanide, in the presence of a hydrosilylation catalyst.

Discussion of the Related Art Fluorosilicon compounds such as cyanoalkyldifluoromethylsilanes and cyanoalkyldimethylfluorosilanes are useful in various applications such as battery fabrication, semiconductor deposition, fluorosilicone glass formation, and semiconductor etching agents. Brief Summary of the Invention One aspect of the invention provides a method of making 3- cyanopropyldimethylfluorosilane, comprising: a reacting tetramethyldisiloxane and boron trifluoride to obtain fluorodimethylsilane; and b reacting fluorodimethylsilane obtained in step a with allyl cyanide.

In another aspect, the invention provides a method of making a cyanoalkyldifluoromethylsilane e. Karstedt's catalyst, which is an organoplatinum compound derived from divinyl-containing disiloxane by treatment of chloroplatinic acid with divinyltetramethyldisiloxane , is an example of a suitable catalyst for this purpose. Other suitable hydrosilylation catalysts include, for example, Wilkinson' s catalyst tris triphenylphosphine rhodium I chloride , the cobalt carbonyl complex Co 2 CO 8, and H 2 PtCl6 Speier's catalyst.

For example, a first portion of the fluorodimethylsilane may be added optionally, in an incremental fashion and the resulting mixture then permitted to react for a period of time before adding a second portion of the fluorodimethylsilane. Synthesis of Cyanoalkyldifluoromethylsilanes A method of making 3-cyanopropyldifluoromethylsilane in accordance with the present invention comprises a step of reacting allyl cyanide and difluoromethylsilane [HSi CH3 F2]. A hydrosilylation catalyst such as, for example, Karstedt' s catalyst, Wilkinson's catalyst tris triphenylphosphine rhodium I chloride , the cobalt carbonyl complex Co 2 CO 8, or H 2 PtCl6 Speier's catalyst may additionally be present to accelerate the rate of reaction.

The present invention further provides, in one aspect, a method of making a cyanoalkyldifluoromethylsilane, comprising a step of reacting a cyanoalkyldichloromethylsilane with ammonium bifluoride. Suitable cyanoalkyldichloromethylsilanes contain, as substituents on the silicon atom, a cyanoalkyl group such as 2-cyanoethyl or 3-cyanopropyl , two chlorine atoms and a methyl group. The fluorination reaction may be carried out by contacting the cyanoalkyldichloromethylsilane with ammonium bifluoride for a time and at a temperature effective to replace the chlorine atoms present in the cyanoalkyldichloromethylsilane with fluorine atoms.

An inert organic solvent capable of forming an azeotrope with water such as toluene may be present in the reaction product mixture; azeotropic distillation of the reaction product mixture to remove water as an azeotrope with the organic solvent may be employed as a method of reducing the water content of the cyanoalkyldifluoromethylsilane that is recovered from the reaction product mixture. Aspects of the present invention including: 1.

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A method of making 3-cyanopropyldimethylfluorosilane, comprising: a reacting tetramethyldisiloxane and boron trifluoride to obtain fluorodimethylsilane; and b reacting fluorodimethylsilane obtained in step a with allyl cyanide. The method of claim 6, wherein the inert solvent is toluene. The method of claim 14, wherein the inert solvent is toluene. The method of any one of claims 23 or 24, wherein the cyanoalkyldichloromethylsilane and ammonium bifluoride are reacted at a molar ratio of from about 0.

Example 4: Synthesis of difluoromethylsilane, DFMS, by reaction of 2,4,6,8- tetramethylcyclotetrasiloxane with BF3 An apparatus and procedure as described in Example 1 was used for Example 4. What is claimed is: 1. A method of making 3-cyanopropyldimethylfluorosilane, comprising:. The method of claim 1, wherein step b is carried out in the presence of a hydrosilylation catalyst. The method of claim 1, wherein fluorodimethylsilane and allyl cyanide are reacted in a molar ratio of from about 0.

The method of claim 1, wherein step b is carried out in the presence of Karstedt' s catalyst. The method of claim 1, wherein step b is carried out in an inert solvent capable of forming an azeotrope with water. The method of claim 6, wherein a reaction product containing 3- cyanopropyldimethylfluorosilane, inert solvent and water is obtained in step b and the reaction product is subjected to distillation wherein water is removed by azeotropic distillation. The method of claim 1, wherein the boron trifluoride is in the form of an etherate complex.

The method of claim 10, wherein the reaction is carried out in an inert solvent capable of forming an azeotrope with water.

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The method of claim 14, wherein a reaction product containing 3- cyanopropyldimethylfluorosilane, inert solvent and water is obtained and the reaction product is subjected to distillation wherein water is removed by azeotropic distillation. The method of claim 17, wherein the allyl cyanide and difluoromethylsilane are reacted in the presence of a hydrosilylation catalyst. The method of claim 17, wherein the allyl cyanide and difluoromethylsilane are reacted at a molar ratio of from about 0. The method of claim 23, wherein the cyanoalkyldichloromethylsilane and ammonium bifluoride are reacted at a molar ratio of from about 0.

The method of claim 23, wherein the reaction is carried out in an inert solvent capable of forming an azeotrope with water. A method of making difluoromethylsilane, comprising reacting a cyclic siloxane and boron trifluoride, wherein the cyclic siloxane contains silicon atoms bearing -H and -CH3 groups as substituents. The method of claim 29, wherein from about 0. USP true USA1 en. EPA4 en.

TWIB en. WOA1 en. Nitrile-substituted silanes and electrolyte compositions and electrochemical devices containing them. Organosilicon heteropolymers and heterocompounds. Physicochemical Characterization of Molecularly Bioengineered Layers. TWA en. EPA1 en. USB2 en.

Lukevit︠s︡, Ė. I︠A︡ (Ėdmund I︠A︡novich)

Tantalum tertiary amylimido tris dimethylamide , a process for producing the same, a solution of starting material for mocvd using the same, and a method of forming a tantalum nitride film using the same. USA en.

RUC2 en. JPB2 en.

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Bis aminoalkyl process for the preparation of polydiorganosiloxane and intermediate products. USB1 en. JPHA en. KRB1 en. Silicone composition crosslinkable into elastomer by hydrosilylation, in the presence of carbene-based metal catalysts, and catalysts.