Synthetic method for high purity triisopropyl silane

A technology of triisopropylsilane and a synthesis method, applied in the direction of silicon organic compounds and the like, can solve the problems of high price, low reactivity, difficult to remove by-product methoxymagnesium chloride, etc., to reduce impurities that are difficult to separate, prevent secondary effect of reaction

Active Publication Date: 2013-07-17
扬州三友合成化工有限公司
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AI Technical Summary

Problems solved by technology

See (PRODUCT-ON OF TRI (SECONDARY ALKYL) SILANE COMPOUND - JP7291977A) for similar reactions. If this kind of reaction is applied to the synthesis of i-Pr3SiH, due to the (OMe)3 is expensi

Method used

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  • Synthetic method for high purity triisopropyl silane
  • Synthetic method for high purity triisopropyl silane

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Experimental program
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Embodiment Construction

[0018] Step 1: Preparation of Isopropylmagnesium Chloride

[0019] In a 500ml four-necked flask equipped with a stirrer, a thermometer and a condenser tube, add 24g (1mol) of metal magnesium, 240g of a solvent (tetrahydrofuran, methyl tetrahydrofuran, ether, propyl ether, n-butyl ether, dioxane , Ethylene glycol dimethyl ether), heat up to reflux, add 78.5g (1mol) of 2-chloropropane dropwise under reflux, keep reflux for 1h, until the metal magnesium is completely dissolved, and the reaction ends.

[0020] Its reaction formula is as follows:

[0021]

[0022] Step 2: Preparation of Triisopropylsilane

[0023] Cool the four-necked flask in step 1 to below 10°C, add 50g of weak polar solvent (xylene, mesitylene, tetrahydronaphthalene, decahydronaphthalene, n-heptane, cyclohexane, methylcyclohexane among them One), under the protection of nitrogen, add 44.72g (0.33 mol) of trichlorosilane dropwise, after the low-temperature dropwise addition, heat up to about 75°C, reflux fo...

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Abstract

The invention discloses a synthetic method for high purity triisopropyl silane, and relates to the technical field of process of preparing triisopropyl silane by a chemical method. The synthetic method comprises the following steps of: performing a reaction on magnesium metal and 2-chloropropane to synthesize isopropyl magnesium chloride; and then, preparing triisopropyl silane at low temperature in presence of a weak polar solvent based on magnesium chloride and trichlorosilane as raw materials. According to the invention, triisopropyl silane is generated by a two-step synthetic method. During preparation of triisopropyl silane, the weak polar solvent which does not affect the solubility of the solvent is used, and the polarity of the solvent is changed to protect side reaction, so as to extremely reduce impurities hard to separate in the reaction process. Finally, high purity triisopropyl silane can be obtained through simple distillation. The product purity can reach 99%.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a new synthesis process of triisopropylsilane. Background technique [0002] Triisopropylsilane is a raw material for synthesizing sterically hindered silicone protective agents. It is mainly used to protect various types of hydroxyl groups, especially in multifunctional hydroxyl compounds, which can be selectively protected and deprotected. It is very important to synthesize nucleosides, nucleotides and sugar compounds; it is also possible to synthesize coatings that can hardly cause capillary cracks and other coating defects even if they are immersed in seawater for a long time, and can prevent or inhibit mucus adhesion, have excellent water resistance and A raw material for an antifouling paint composition that can effectively produce a coating film with an antifouling effect over a long period of time, which reduces the content of volatile organic compounds (VOC) that evaporate ...

Claims

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Application Information

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IPC IPC(8): C07F7/08
Inventor 魏开举李辉宁张扬李明成张才山
Owner 扬州三友合成化工有限公司
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