Method of preparing hexamethyldisilane amine sodium solution

A technology of sodium hexamethyldisilazide and hexamethyldisilazine, which is applied in the field of preparation of sodium hexamethyldisilazide tetrahydrofuran solution, and can solve the problems of low reaction yield and long reaction time

Inactive Publication Date: 2009-07-29
SHAANXI DASHENG PHARMA TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Strict requirements on solvent anhydrous,...

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0016] In a 500ml three-necked flask, add 100g (0.62mol) of hexamethyldisilazane amine, add 20g (0.5mol) of 60% (w / w) sodium hydride under stirring, heat in an oil bath at 110-115°C for 3 hours, cool Zone to below 50°C, add 120g of anhydrous tetrahydrofuran to dissolve, and let stand to precipitate. Take the supernatant to test the content, and the solution contains 89.5 g (0.49 mol) of sodium hexamethyldisilazide. The yield is 98% based on sodium hydride.

Embodiment 2

[0018] In a 1000ml three-necked flask, add 300g of anhydrous toluene, add 322.8g (2.0mol) of hexamethyldisilazane under stirring, add 82.0g (2.05mol) of 60% (w / w) sodium hydride, heat to reflux, reflux The temperature was 110-115°C, and the reaction was kept under reflux for 4 hours. Cool to 40-50°C, add 300 g of dry tetrahydrofuran, and stir until dissolved. Let the precipitation stand, and take the supernatant to test the content. The solution contains 356 g (1.96 mol) of sodium hexamethylsilylamine. The yield based on sodium hydride is 95.6%.

Embodiment 3

[0020] In a 1000ml three-neck flask, add 300g of anhydrous toluene, add 322.8g (2.0mol) of hexamethyldisilazane under stirring, add 90.0g (2.25mol) of 60% (w / w) sodium hydride, heat to reflux, reflux The temperature was 110-115°C, and the reaction was kept under reflux for 4 hours. Cool to 40-50°C, add 300 g of dry tetrahydrofuran, and stir until dissolved. Let the precipitation stand, and take the supernatant to test the concentration. The solution contains 361 g (1.97 mol) of sodium hexamethylsilylamine. The reaction yield is 87.5% based on sodium hydride.

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Abstract

The invention provides a preparation method of hexamethyldisilane sodium amine solution which is characterized in that hexamethyldisilazane and sodium hydride react with each other in high boiling point solvent or without solvent. When the reaction is finished completely, tetrahydrofuran is used for the dissolution to obtain hexamethyldisilane sodium amine tetrahydrofuran solution, wherein, the mol ratio of the hexamethyldisilazane to the sodium hydride is 1.0 to 0.8-1.2. The sodium hydride is oil dispersed sodium hydride with the content of 60-70 percent and the reaction temperature of 80-130 DEG C. The reaction temperature in the high boiling point solvent is the reflux temperature, and the reaction time is 3-4 hours of the reflux state. Shown by detection and organic synthesis tests, the preparation method adopted by the invention has the advantages of simplicity, fast reaction speed and completeness of reaction.

Description

Technical field: [0001] The invention relates to a preparation method of sodium hexamethyldisilazane amine solution, in particular to a preparation method of hexamethyldisilazane sodium tetrahydrofuran solution. Background technique: [0002] Sodium hexamethyldisilazane tetrahydrofuran solution is a strong base catalyst used in organic synthesis. The hexamethylsilylamine sodium tetrahydrofuran solution was used to prepare the synthesis of the intermediate of the drug Mitiglunude, and achieved satisfactory results. [0003] The usual preparation method is that hexamethyldisilazylamine and sodium hydride are refluxed in anhydrous tetrahydrofuran for a long time. The specific synthesis method is: under the protection of nitrogen, add sodium hydride to anhydrous tetrahydrofuran, add hexamethyldisilazane amine dropwise under stirring, reflux for 12 hours, let it stand for precipitation, and the supernatant is the prepared hexamethyldisilazane Sodium silylamine tetrahydrofuran s...

Claims

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Application Information

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IPC IPC(8): C07F7/10C07F1/04
Inventor 贺向民
Owner SHAANXI DASHENG PHARMA TECH
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