A kind of method of lithium hydride selective reduction chloroalkyl chlorosilane

A technology of chloroalkylchlorosilane and chloroalkylhydrosilane, which is applied in the field of selective reduction of chloroalkylchlorosilane by lithium hydride, can solve the problems that the rapid and efficient selective reduction of chloroalkylchlorosilane cannot be achieved, and achieve the reduction reaction The effect of fast rate, high yield and mild reaction conditions

Active Publication Date: 2019-06-07
INST OF CHEM CHINESE ACAD OF SCI
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Problems solved by technology

[0009] In view of the above analysis, the present invention aims to provide a method for the selective reduction of chloroalkyl chlorosilanes by lithium hydride, which solves the problem that in the prior art, chloroalkyl chlorosilanes cannot be quickly and efficiently selectively reduced to prepare chloroalkyl silanes. Hydrosilane Problems

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  • A kind of method of lithium hydride selective reduction chloroalkyl chlorosilane
  • A kind of method of lithium hydride selective reduction chloroalkyl chlorosilane
  • A kind of method of lithium hydride selective reduction chloroalkyl chlorosilane

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preparation example Construction

[0048] Specifically, the preparation method of above-mentioned chloroalkyl hydrosilane comprises the following steps:

[0049] Step S1: under anhydrous conditions and under the protection of an inert gas, mix lithium hydride, catalyst and ether solvent, and stir evenly to obtain a mixed solution of lithium hydride and catalyst;

[0050] Step S2: Under stirring, add chloroalkylchlorosilane dropwise to the mixed solution of lithium hydride and catalyst, carry out the reduction reaction at 0°C-140°C for 0.1h-24h, and the reaction product is separated and purified (for example, distillation) Finally, the corresponding chloroalkylhydrosilanes are obtained.

[0051] Above-mentioned chloroalkyl chlorosilane can be ClPrSiMeCl 2 , ClCH 2 SiMeCl 2 , ClCH 2 SiMe 2 Cl, Cl 2 CHSiMeCl 2 , ClCH 2 SiCl 3 , ClCH 2 CH 2 SiMeCl 2 or Cl 2 CHSiCl 3 . It can be seen from this that the above method for preparing chloroalkylhydrosilanes can be applied to the reduction reaction of vario...

Embodiment 1

[0060] The 250mL three-neck round bottom flask was dried, connected with a mechanical stirrer, spherical condenser, constant pressure funnel, and gas guiding device, and then evacuated for three times to replace nitrogen, and at the same time baked with a heat gun to remove attached water vapor. Under a nitrogen atmosphere, add 1.8g (0.22mol) LiH, 0.022g (0.001mol) LiBH to the reaction flask 4 , 20mL tetrahydrofuran solvent, and control the reaction temperature at 30-40°C. Add 16.7g (0.1mol) ClCH to the constant pressure funnel 2 SiMeCl 2 , slowly dropwise into the reaction flask under mechanical stirring. Continue to stir the reaction for 1h after the dropwise addition, the reduction product is ClCH 2 SiMeH 2 , the yield was 100%.

[0061] The method of the present embodiment is reacted to the product, raw material and solvent in the final system 1 H-NMR spectrum as figure 2 shown.

Embodiment 2

[0067] The 250mL three-neck round bottom flask was dried, connected with a mechanical stirrer, a spherical condenser, a constant pressure funnel and a 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, add 2.7g (0.33mol) LiH, 0.022g (0.001mol) LiBH to the reaction flask 4 , 20mL tetrahydrofuran solvent. Add 18.4g (0.1mol) ClCH to the constant pressure funnel 2 SiCl 3 , slowly added dropwise into the reaction flask under mechanical stirring, keeping the reaction temperature between 30 and 40°C. After the dropwise addition was completed, the reaction was continued for 1 h to obtain the product ClCH 2 SiH 3 , the yield was 100%.

[0068] The method of the present embodiment is reacted to the product, raw material and solvent in the final system 1 H-NMR spectrum as Figure 4 shown.

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Abstract

The invention discloses a method used for selective reduction of chlorine alkylchlorosilane with lithium hydride, and belongs to the technical field of chlorine alkylchlorosilane reduction. The methodis capable of solving a problem in the prior art that it is impossible to prepare chlorine alkyl hydrosilane through rapid high efficiency selective reduction of chlorine alkylchlorosilane. Accordingto the method, in an ether solvent, under the effect of a catalyst, lithium hydride is taken as a reducing agent, chlorine alkylchlorosilane is reduced into chlorine alkyl hydrosilane; a borane, a hydroboron, or lithium aluminium hydride is taken as a catalyst; the molar ratio of the catalyst to lithium hydride is controlled to be 1:41-100000. The method can also used for preparation of chlorinealkyl hydrosilane through reduction of chlorine alkylchlorosilane.

Description

technical field [0001] The invention relates to a reduction of chloroalkylchlorosilanes, in particular to a method for selectively reducing chloroalkylchlorosilanes with lithium hydride. 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
CPCC07F7/126
Inventor 李永明陈义徐彩虹王新良
Owner INST OF CHEM CHINESE ACAD OF SCI
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