A kind of preparation method of iodotrimethylsilane

A technology of iodotrimethylsilane and hexamethyldisiloxane, which is applied in the field of preparation of iodotrimethylsilane, can solve problems such as complex process, low yield, and difficult product purification, and achieve simple purification and high yield High, less impurity effect

Active Publication Date: 2017-09-29
佛山市南海区波尔有机硅有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the defects of low yield, difficult product purification and complicated process in the above-mentioned existing method for preparing iodotrimethylsilane, and provide a trimethyl iodosilane with high product yield, simple purity and warm reaction conditions. The preparation method of methyl iodosilane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of iodotrimethylsilane, the method may further comprise the steps:

[0023] 250ml three-neck flask, device addition funnel, nitrogen conduit and reflux condenser, open nitrogen purge, add anhydrous aluminum trichloride 17.3g (130mmol, average particle diameter is 85μm) and hexamethyldisiloxane 16.2g (100mmol ), start magnetic stirring, heat up to 40°C, then add 88.8g (350mmol, each 29.6g) of elemental iodine three times through the addition funnel, each time of addition is 5 minutes, and the bath temperature rises to 120°C after the addition of elemental iodine is completed , The reaction was refluxed for 1 hour, the device was changed to a distillation device, and the distillate was collected at 106-107 ° C to obtain 39 g of iodotrimethylsilane with a purity of 99.8% and a yield of 97.4%.

Embodiment 2

[0025] A preparation method of iodotrimethylsilane, the method may further comprise the steps:

[0026] 250ml three-neck flask, device addition funnel, nitrogen conduit and reflux condenser, open nitrogen purge, add anhydrous aluminum trichloride (120mmol, average particle diameter is 100μm) and hexamethyldisiloxane 16.2g (100mmol), Start magnetic stirring, be warming up to 45 ℃, then add 104.4g (400mmol, each 33.8g) of elemental iodine three times through the addition funnel, each feeding time is 8 minutes, and the bath temperature rises to 125 ℃ after the addition of elemental iodine is completed, and the reaction Reflux for 1.2 hours, change the device to a distillation device, and distill at atmospheric pressure to collect fractions at 106-107°C to obtain 38.6 g of iodotrimethylsilane with a purity of 99.8% and a yield of 96.7%.

Embodiment 3

[0028] A preparation method of iodotrimethylsilane, the method may further comprise the steps:

[0029] A 250ml three-neck flask, equipped with an addition funnel, a nitrogen conduit and a reflux condenser, opened the nitrogen purge, added anhydrous aluminum trichloride (125mmol average particle size of 75μm) and hexamethyldisiloxane 16.2g (100mmol), and started Magnetic stirring, heating up to 50°C, then adding 91.5g (360mmol, 30.5g each time) of iodine elemental substance three times through the addition funnel, each addition time is 7 minutes, after the addition of elemental iodine substance, the bath temperature rises to 130°C, and the reaction is refluxed For 1 hour, the device was changed to a distillation device, distilled at atmospheric pressure, and the fraction at 106-107°C was collected to obtain 38.6 g of iodotrimethylsilane with a purity of 99.5% and a yield of 96.4%.

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Abstract

The invention discloses a preparation method of iodotrimethylsilane, which comprises: adding anhydrous aluminum chloride and hexamethyldisiloxane into a reaction vessel in the presence of a protective gas, starting to stir, and raising the temperature to 40‑50°C, then add iodine elemental substance, after the addition of iodine elemental substance, the bath temperature rises to 125‑140°C, and the reaction is refluxed for 1‑1.5 hours. Methyl iodosilane. The method can improve the yield of iodotrimethylsilane, has simple purification, mild conditions, and is suitable for large-scale production and popularization.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method of iodotrimethylsilane. 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 cefepime. , Application in the synthesis of cefpirome. [0003] At present, there are many ways to synthesize iodotrimethylsilane. The commonly used synthesis method in industry is to react hexamethyldisiloxane with iodine and aluminum powder to prepare iodotrimethylsilane. Most of the iodotrimethylsilane sold in the market adopts the above-mentioned method, and the iodotrimethylsilane prepared by this method contains many impurities such as low-boiling substances (such as tetramethylsilane ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
Inventor 孟凡军任井斌倪萍
Owner 佛山市南海区波尔有机硅有限公司
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