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Method for catalytically synthesizing silanol

A technology of silanol and catalyst, which is applied in the field of catalyzing synthesis of silanol compounds with water as an oxidant copper salt, can solve the problems of unsuitability for large-scale production, low selectivity, narrow application range, etc., and achieves easy separation and simple product separation method. , the effect of less emission of "three wastes"

Inactive Publication Date: 2014-07-16
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of this catalytic reaction process is that the scope of application is narrow, and disiloxane by-products will be formed during the reaction process, resulting in low selectivity
[Motokura K.; Kashiwame D.; Miyaji, A.; Baba, T.Org.Lett.2012, 14, 2642.] and the operation is cumbersome, not suitable for large-scale production

Method used

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  • Method for catalytically synthesizing silanol
  • Method for catalytically synthesizing silanol
  • Method for catalytically synthesizing silanol

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Mix triethylsilane 1a (2mmol) with water (2mmol), use copper sulfate as a catalyst, the catalyst dosage is 1mol% of the moles of triethylsilane, react in the air without solvent, stir and heat to 50°C, and the reaction time is 3 hours. After the reaction, 20 mL of water was added, extracted with ethyl acetate, dried, and the solvent was distilled off under reduced pressure to obtain colorless liquid triethylsilanol 1b. The conversion of silane was 100%, and the yield of triethylsilanol 1b was 93%.

Embodiment 2

[0028] Mix trihexylsilane 2a (2mmol) with water (2mmol), add copper sulfate as a catalyst, the amount of catalyst is 1mol% of the moles of trihexylsilane, react in the air without solvent, stir and heat to 50°C, and the reaction time is 3 hours . After the reaction, 10 mL of water was added, extracted with ethyl acetate, dried, and the solvent was distilled off under reduced pressure to obtain trihexylsilanol 2b as a colorless liquid. The conversion of silane was 100%, and the yield of trihexylsilanol 2b was 91%.

Embodiment 3

[0030] Mix triisopropylsilane 3a (2mmol) with water (2mmol), add copper oxide as a catalyst, the catalyst dosage is 10mol% of the moles of triisopropylsilane, react without solvent under air, stir and heat to 50°C, react The time is 3 hours. After the reaction, 15 mL of water was added, extracted with ethyl acetate, dried, and the solvent was distilled off under reduced pressure to obtain colorless liquid triisopropylsilanol 3b. The conversion of triisopropylsilane was 100%, and the yield of triisopropylsilanol 3b was 93%.

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Abstract

The invention discloses a method for catalytically synthesizing silanol and relates to the fields of organic chemicals and fine chemicals. The method is essentially a transition metal catalyzed organic synthesis reaction. In the method, the raw materials comprise organosilane and a clean oxidant, a used catalyst is inexpensive copper salt, the raw material is heated and stirred to react without a solvent so as to rapidly produce silanol at a moderate temperature. By adopting the method, the reaction time is 3-12 hours. The mole ratio of the organosilane to the clean oxidant is 1:(1-5), the copper salt as the catalyst accounts for 1-10mol% of the mole number of the organosilane, the raw materials react at a temperature of 50-80 DEG C, and then the silanol can be greatly yielded after simple posttreatment. The oxidant used in the method is safe and nontoxic, and the catalyst used in the method is cheap and easily available. The method disclosed by the invention is a very simple and practical method for synthesizing silanol.

Description

technical field [0001] The invention relates to the fields of organic chemical industry and fine chemical industry, in particular to a method for catalytically synthesizing silanol compounds with water as an oxidant copper salt. Background technique [0002] In recent years, the research on organic silicon alcohol compounds has gradually increased. Silanols can not only be used as universal reaction building blocks in organic synthesis, but also important raw materials for the synthesis of silicon-containing polymer materials in industrial production. . Not only that, silanol compounds are also widely used in the research of organic synthetic chemistry and pharmacology. [0003] The traditional methods of synthesizing silanols can be roughly divided into three categories: the hydrolysis reaction of chlorosilanes, the action of strong bases and silane ethers, and the oxidation reaction of silanes. Since silane compounds are relatively common and easy to synthesize, and the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C07F7/04C07F7/12
Inventor 于金涛郭欢朱卉成江
Owner CHANGZHOU UNIV
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