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Preparation method of high purity tert-butyl alcohol magnesium

A magnesium tert-butoxide, high-purity technology, applied in the direction of metal alcohol preparation, sustainable manufacturing/processing, chemical industry, etc., can solve the problem of low solubility

Inactive Publication Date: 2010-06-09
SHANGHAI AURISCO INT TRADING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Studies have found that the solubility of magnesium tert-butoxide in the reaction system is too low, resulting in the formation of magnesium tert-butoxide in the alcohol exchange reaction process, which is quickly saturated and precipitated in the reaction mixture, trapping unreacted magnesium methoxide and failing to remove methanol in time , this part of magnesium methylate no longer participates in the reaction and remains in magnesium tert-butoxide all the time, causing the purity of final magnesium tert-butoxide to only reach 70%.

Method used

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  • Preparation method of high purity tert-butyl alcohol magnesium

Examples

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Effect test

Embodiment 1

[0024] Get 1800g tert-butyl acetate and place in 2000ml four-neck flask with stirring, and the reaction bottle device has a precision rectifying column with an internal diameter of 15 millimeters and a height of 800 millimeters, N 2 Heated to 95° C. under protection, and added 409 g of 14.1% magnesium methoxide methanol solution at a rate of 15 ml / min, and a white precipitate appeared at the beginning. After the dropwise addition, the kettle temperature was 95°C, and the overhead distillation temperature was 57°C, and the reflux ratio was set to be 1 at this time. With the gradual distillation of methyl acetate and the gradual increase of the temperature of the kettle, the temperature of the overhead distillation also increases, and gradually rises from 57°C to 97°C. At this time, the overhead liquid does not contain methyl acetate. Esters, all tert-butyl acetate. At the same time, the reflux ratio was adjusted to 5 and finally to 20 as the temperature at the top of the tower...

Embodiment 2

[0026] Get 600g tert-butyl acetate and place in 1000ml four-necked flask with stirring, and the reaction bottle device has a precision rectifying column with an internal diameter of 15 millimeters and a height of 800 millimeters, N 2 Under protection, add 50 g of solid magnesium methoxide, heat the suspension to reflux, and reflux for 2 hours. When the temperature at the top of the tower is 57° C., set the reflux ratio to 5. With the gradual distillation of methyl acetate, the temperature of the overhead distillation also increases, and gradually rises from 57°C to 97°C. At this time, the overhead liquid does not contain methyl acetate, and all of it is tert-butyl acetate. ester. At the same time, the reflux ratio was adjusted to 20 with the gradual increase of the tower top temperature. After a long period of time (1 hour) when the temperature at the top of the tower was stable at 97° C., the distillation was stopped, and the reaction time required about 8 hours. The rectif...

Embodiment 3

[0028] Get 500g tert-butyl acetate and place in a four-necked flask with stirring of 1000ml, and the reaction bottle device has a precision rectification column with an internal diameter of 15 mm and a height of 800 mm, N 2 Under protection, add 65 grams of solid magnesium ethoxide, heat the suspension to reflux, and reflux for 2 hours. When the temperature at the top of the tower is 77° C., set the reflux ratio to 10. With the gradual distillation of ethyl acetate, the temperature of the overhead distillation also increases, and gradually rises from 77°C to 97°C. At this time, the overhead liquid does not contain ethyl acetate, but is all tert-butyl acetate ester. At the same time, the reflux ratio was adjusted to 20 with the gradual increase of the tower top temperature. After a long period of time (1 hour) when the tower top temperature is stable at 97° C., the distillation is stopped, and the reaction time takes about 10 hours. The rectification device was changed to a v...

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Abstract

The invention discloses a preparation method of high purity tert-butyl alcohol magnesium. Transfer esterification is carried out on low level alkyl radical magnesium alkoxide and tert butyl alcohol ester in case of reactive rectification (or distillation), thus obtaining high purity tert-butyl alcohol magnesium. The purity of tert-butyl alcohol magnesium prepared by the method of the invention reaches 92-98%.The method is simple and convenient, features high yield and suitability for industrialized production.

Description

Technical field: [0001] The present invention relates to medicinal chemistry. It specifically relates to a preparation method of high-purity magnesium tert-butoxide. Background technique: [0002] Magnesium alcohol compound is a kind of metal alcohol compound, its molecular structure is Mg(OR) 2 , R = alkyl. It is a water-sensitive solid and is mainly used as a selective base in organic synthesis, as a neutralizer in anhydrous systems, as a raw material for preparing high-purity magnesium oxide, as a chemical intermediate and as a catalyst carrier for polyolefins. Since divalent metal magnesium ions can form stable chelates with carbonyl groups, magnesium alcohol compounds such as magnesium methoxide can be used as selective carbonyl coagulants. In recent years, with the rapid development of the metal alkoxide sol-gel method, magnesium alkoxide compounds have also been used in many ways, and their potential application prospects are also attracting attention. [0003] Ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/30C07C29/68
CPCC07C29/68Y02P20/10C07C31/30
Inventor 俞迪虎
Owner SHANGHAI AURISCO INT TRADING
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