Preparation method of tris(trimethylsilyl)phosphite

A technology of trimethylsilyl and phosphite, which is applied in the field of preparation of high-purity triphosphite, can solve the problems of slow reaction speed, unsatisfactory, harsh application, etc., and achieve rapid reaction, high product quality and simple separation Effect

Inactive Publication Date: 2016-10-26
ZHENJIANG SINOWA POLYURETHANE EQUIP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In summary, the prior art has the following disadvantages: the reaction rate is slow, and it needs to be refluxed for 20 hours before the selectivity of the target product (1) can reach 70%; the reaction process is controlled by equilibrium, and the by-product (2) in the system cannot be completely Converted into the target product (1); in the follow-up product separation and purification process, the recovery of the by-product (2) needs to be considered; only relying on filtration can not completely remove triethylamine hydrochloride, so in the follow-up product separation process, the volatile Stronger triethylamine hydrochloride makes industrialized continuous production be difficult to realize; Both boiling point difference is little (under 20mmHg vacuum tightness, boiling point difference is less than 20 ℃) ​​in the vacuum rectification process, by product (2) to target product (1 ) purification caused some interference; the highest purity of products sold in the market is 98%, and there are no high-purity products above 99%
Not suitable for more demanding applications

Method used

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  • Preparation method of tris(trimethylsilyl)phosphite

Examples

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Effect test

Embodiment 1

[0022] Example 1: Select tetrahydrofuran as the solvent, add potassium trimethylsiliconate and phosphorus trichloride to the above solvent at a molar ratio of 1:1, stir vigorously during the addition, and filter to remove the chloride Potassium, the above solution is distilled under reduced pressure at 90°C / 20mmHg to obtain the target product, and the purity of the target product can reach more than 99.8%.

Embodiment 2

[0023] Example 2: Select tetrahydrofuran as the solvent, add potassium trimethylsiliconate and phosphorus tribromide to the above solvent at a molar ratio of 1:1, stir vigorously during the addition, and filter to remove the bromide Potassium, the above solution is distilled under reduced pressure at 90°C / 20mmHg to obtain the target product, and the purity of the target product can reach more than 99.7%.

Embodiment 3

[0024] Example 3: Select tetrahydrofuran as the solvent, add sodium trimethylsiliconate and phosphorus trichloride to the above solvent at a molar ratio of 1:1, stir vigorously during the addition, and filter to remove the chloride Sodium, the above solution is distilled under reduced pressure at 90°C / 20mmHg to obtain the target product, and the purity of the target product can reach more than 99.7%.

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Abstract

The invention discloses a preparation method of tris(trimethylsilyl)phosphate. The preparation method comprises the steps that an alkane or ether solvent is selected, two reactants including alkali metal silicon alkoxide and phosphorus halide are added into the solvent according to the mole ratio of 1:1, and stirring is intensely conducted in the adding process; inorganic salt is removed through filtration, and reduced pressure distillation is conducted on the solution under the condition of 90 DEG C / 20 mmHg to obtain the target product, wherein the purity of the product can reach 99.6% or above. Accordingly, industrialized production is achieved, and great market prospects and economic values are achieved.

Description

technical field [0001] The invention relates to a preparation method for high-purity tris(trimethylsilyl)phosphite. Background technique [0002] Tris(trimethylsilyl)phosphite is a commonly used pharmaceutical intermediate and organic reagent, mainly used in the synthesis of special alkenes or alkynes. At present, there is no mass-scale industrial production method in China, and it mainly relies on imports. The bulk import price of reagent-grade products is about 30,000 yuan / kg, while the maximum package price in the retail market is about 10,000 yuan / 100g. [0003] From the published reports, the only synthetic preparation method at present is the preparation method of using trimethylchlorosilane and phosphorous acid reaction in the presence of triethylamine and common solvents (such as tetrahydrofuran, cyclohexane, etc.), specifically The reaction mechanism refers to the following reaction equation: [0004] [0005] Wherein, triethylamine plays the role of hydrogen ...

Claims

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Application Information

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IPC IPC(8): C07F9/141
CPCC07F9/1415
Inventor 徐应刚
Owner ZHENJIANG SINOWA POLYURETHANE EQUIP
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