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Novel method for preparing trimethyliodosilane

A technology of trimethyl iodide silane and trimethyl chlorosilane, applied in the field of chemical synthesis, can solve the problems of complicated operation process, difficult operation, unsafety and the like, and achieve the effect of simple and safe process, easy operation and easy operation

Active Publication Date: 2017-07-07
山东博苑医药化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the invention of the present invention is to solve the unsafe problem of adding iodine in batches in the prior art; the unsafe problem of using high-risk chemical metal sodium potassium; complex operation process, difficult operation, low yield, more three wastes, etc. question

Method used

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  • Novel method for preparing trimethyliodosilane

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Effect test

Embodiment 1

[0035] Experimental conditions: a) The molar ratio of anhydrous lithium chloride to anhydrous sodium iodide is 1:1, and the reaction temperature is 60°C; b) When iodosilane is synthesized, the ratio of lithium iodide to trimethylchlorosilane is 1: 2. The reaction temperature is 60°C, and the catalyst dosage is 2.5%.

[0036] (1) Preparation of anhydrous lithium iodide: add 107.32g sodium iodide (molar ratio 1:1) in portions to the 300ml acetone solution of 30.29g lithium chloride, react for 1 hour after dripping; Sodium chloride was removed; the filtrate was concentrated and evaporated to dryness to obtain lithium iodide, and after drying, 94 g (98.04%) of anhydrous lithium iodide was obtained, with a yield of 96%. The evaporated acetone is recovered and recycled after water removal.

[0037](2) Preparation of iodotrimethylsilane: place 94g lithium iodide, 154.78g trimethylchlorosilane (molar ratio 1:2) and 2.5% catalyst tetrabutylammonium iodide in a reaction flask under a n...

Embodiment 2

[0040] Experimental conditions: Example 1 reclaims lithium iodide and the recycling of trimethylchlorosilane, and other conditions are the same as Example 1. It is verified that recycling of materials can improve the yield of trimethyliodosilane, but has no effect on product quality.

[0041] (1) Preparation of iodotrimethylsilane: Lithium iodide 92g prepared by reclaiming lithium chloride in Example 1, 73.58g new trimethylchlorosilane, 77.57g example one steamed trimethylchlorosilane fraction and chlorine After washing with lithium chloride, the mother liquor of trimethylchlorosilane and 2.5% catalyst tetrabutylammonium iodide are placed in a reaction flask, under a nitrogen atmosphere, and reacted at a certain temperature for 10 hours to obtain a crude product of iodotrimethylsilane, which is obtained after rectification The finished product of iodotrimethylsilane is 133.22g, the purity is 99.32%, and the yield is 98.56%.

[0042] (2) recycling of lithium chloride: prepare 3...

Embodiment 3

[0044] Experimental conditions: a) The molar ratio of anhydrous lithium chloride to anhydrous sodium iodide is 1.05:1, and the reaction temperature is 60°C; b) When iodosilane is synthesized, the ratio of lithium iodide to trimethylchlorosilane is 1: 1.2, the reaction temperature is 60°C, and the catalyst consumption is 2.5%.

[0045] (1) Preparation of anhydrous lithium iodide: Add 151.19 g of sodium iodide (1.05:1) in portions to 44.81 g of lithium chloride in acetone, and react for 1 hour after the drop; after the reaction is completed, filter out the chloride Sodium; the filtrate was concentrated and evaporated to dryness to obtain lithium iodide, and after drying, 134.12 g (97.80%) of anhydrous lithium iodide was obtained, with a yield of 98%. The evaporated acetone is recovered and recycled after water removal. The feed ratio of anhydrous lithium chloride to anhydrous sodium iodide is 1.05:1, and the conversion rate of lithium iodide is improved compared with Example 1....

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Abstract

The invention relates to a preparation process of trimethyliodosilane, which has the advantages of moderate reaction conditions, simple process, safety in operation, high yield and extremely few three wastes. The preparation process takes anhydrous sodium iodide, anhydrous lithium chloride and trimethylchlorosilane as raw materials and the raw materials react in a dried nitrogen atmosphere to synthesize the trimethyliodosilane. According to the method provided by the invention, a traditional complicated process of preparing trimethyliodosilane from hexamethyldisilane and hexamethyldisiloxane is changed; reaction conditions are moderate and operation is safe; dangers of utilizing high-danger chemicals including metal potassium and sodium are avoided; meanwhile, a high-temperature iodization difficulty is also avoided; in a whole production circulating process, only the trimethyliodosilane product and a byproduct sodium chloride are produced and other three wastes are not generated, so that the process is green and environmental-friendly.

Description

technical field [0001] The invention relates to a method for preparing chemical products, in particular to a new method for preparing iodotrimethylsilane, which belongs to the field of chemical synthesis. Background technique [0002] Iodotrimethylsilane is often used as a protective reagent for functional groups such as amino, hydroxyl, and mercapto groups in the field of drug synthesis and organic synthesis. Due to its high activity and mild reaction conditions, it has a wide range of applications, especially in drug synthesis, such as In the synthesis of cefepime and cefpirome. Commercially available iodotrimethylsilane contains a lot of low-boiling impurities (such as tetramethylsilane and dimethyldiiodosilane), and this impurity-containing product is not conducive to the synthesis of cephalosporins, and may also form post-medication side effect. At present, there are more than 10 synthetic methods of iodotrimethylsilane, and the more practical and industrialized synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12
CPCC07F7/123
Inventor 李成林汪清民翟永利楚荣强
Owner 山东博苑医药化学股份有限公司
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