Preparation method of chloride alkyl hydrogen silane

A technology of chloroalkylhydrosilane and chloroalkylchlorosilane, which is applied in the field of preparation of chloroalkylhydrosilane, can solve problems such as the inability to selectively reduce chloroalkylhydrosilane with chloroalkylchlorosilane, and achieve easy recycling , fast reaction rate and high yield

Active Publication Date: 2018-06-08
INST OF CHEM CHINESE ACAD OF SCI
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Problems solved by technology

[0008] In view of the above analysis, the present invention aims to provide a method for the preparation of chloroalkylhydrosilanes, which solves the problem that in the prior art, chloroalkylchlorosilanes cannot be quickly and efficiently selectively reduced to prepare chloroalkylhydrosilanes. The problem

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  • Preparation method of chloride alkyl hydrogen silane
  • Preparation method of chloride alkyl hydrogen silane
  • Preparation method of chloride alkyl hydrogen silane

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[0033] The invention provides a preparation method of chloroalkylhydrosilane. In an ether solvent, under the catalysis of a catalyst, LiH is used as a reducing agent to reduce chloroalkylchlorosilane to chloroalkylhydrosilane; wherein, the catalyst For borane, borohydride or lithium aluminum hydride.

[0034] The experimental route is as follows:

[0035]

[0036] Among them, R 1 , R 2 Represents the same or different alkyl, halogen and other groups; R C Represents a chloroalkyl group in which C-H on the alkyl group is replaced by one or more Cl.

[0037] Compared with the prior art, the preparation method of chloroalkylhydrosilane provided by the present invention adopts LiH with lower cost as reducing agent, borane, borohydride and lithium aluminum hydride as catalyst, and ether solvent as reaction Solvent, can realize the selective reduction of chloroalkylchlorosilane, only reduce silicon-chlorine bond and retain carbon-chlorine bond, prepare chloroalkylhydrosilane c...

Embodiment 1

[0053] The 250mL three-neck round bottom flask was dried, connected with a spherical condenser, constant pressure funnel and gas guiding device, vacuumed three times to replace nitrogen, and at the same time baked with a hot air gun to remove attached water vapor. Under nitrogen atmosphere, add 1.8g (0.22mol) LiH, 20mL tetrahydrofuran solvent, 2ml borane dimethyl sulfide solution ((CH 3 ) 2 S·BH 3 ) (10mol / L). Add 19.2g (0.1mol) ClCH to the constant pressure funnel 2 CH 2 CH 2 SiMeCl 2 , slowly dropwise into the reaction flask under magnetic stirring. After the dropwise addition was completed, react at room temperature for 5 h to obtain the product ClCH 2 CH 2 CH 2 SiMeH 2 , the yield was 90%.

Embodiment 2

[0055] The 250mL three-neck round bottom flask was dried, connected with a spherical condenser, constant pressure funnel and gas guiding device, vacuumed three times to replace nitrogen, and at the same time baked with a hot air gun to remove attached water vapor. Under a nitrogen atmosphere, 1.8 g (0.22 mol) of LiH, 20 mL of tetrahydrofuran solvent, and 20 ml of borane tetrahydrofuran solution (1 mol / L) were added to the reaction flask. Add 17.8g (0.1mol) ClCH to the constant pressure funnel 2 CH 2 SiMeCl 2 , slowly dropwise into the reaction flask under magnetic stirring. After the dropwise addition, react at room temperature for 10 h to obtain the product ClCH 2 CH 2 SiMeH 2 , the yield was 85%.

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Abstract

The invention discloses a preparation method of chloride alkyl hydrogen silane, belongs to the technical field of reduction of the chloride alkylchlorosilane, and solves the problem that in the priorart, the chloride alkyl hydrogen silane cannot be prepared through selective reduction of the chloride alkyl chlorosilane. In an ether solvent, under the catalysis of a catalyst, LiH is adopted as a reducing agent, the chloride alkyl chlorosilane is reduced to the chloride alkyl hydrogen silane; the catalyst is boron hydride, borohydride or lithium aluminum hydride. The preparation method can be used for preparing the chloride alkyl hydrogen silane.

Description

technical field [0001] The invention relates to the reduction of chloroalkylchlorosilanes, in particular to a preparation method of chloroalkylhydrosilanes. Background technique [0002] Chloroalkyl hydrosilane is an organosilicon compound with silicon-hydrogen bond in its molecule and chloroalkyl group attached to the silicon atom. Because it has both chloroalkyl and silicon-hydrogen bond functional groups, many novel organosilicon compounds and their polymers can be synthesized using chloroalkylhydrosilanes. [0003] In the prior art, the preparation method of chloroalkylhydrosilane mainly adopts the reduction method, that is, the reaction of chloroalkylchlorosilane with abundant sources and a strong reducing agent is used to reduce all or part of the chlorine on the silicon atom to H, and retain the chlorine The alkyl group is not reduced to give the chloroalkylhydrosilane. [0004] LiAlH 4 It has strong reducing ability, and can complete many reduction reactions with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
CPCC07F7/0896
Inventor 李永明陈义徐彩虹耿金垚王新良
Owner INST OF CHEM CHINESE ACAD OF SCI
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