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Synthetic method of neopentyl alcohol of high purity

A synthesis method and technology of neopentyl alcohol, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of high overall cost, complicated reaction operation, and inability to meet the needs of high-end products.

Inactive Publication Date: 2014-03-19
ZHANGJIAKOU SIRUIKAI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is reported that pivaloyl chloride reduction method is used to prepare neopentyl alcohol. The catalyst used in this method is tetramethylethylenediamine (TMEDA), which is expensive and uses a large amount and cannot be recycled. The cost of the product will be greatly increased when the scale-up production is carried out.
2: Reduction of pivalaldehyde: Tetrahedron Letters, 50(37), 5270-5273, 2009 reported the method of preparing neopentyl alcohol by reduction of pivalaldehyde. Although the yield is high, the expensive catalyst PtO2 is used, and the raw material Difficult to prepare, the overall cost is too high
The reaction needs to be protected by inert gas, the reaction operation is complicated, and the product purity is only 98%, which cannot meet the needs of some high-end products
[0009] Some of the finished products synthesized by the above methods have many impurities, which cannot meet the needs of some high-end products
Although some can increase the content of the product, the higher cost is not conducive to the promotion and production of industrialization

Method used

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  • Synthetic method of neopentyl alcohol of high purity
  • Synthetic method of neopentyl alcohol of high purity
  • Synthetic method of neopentyl alcohol of high purity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0017] Example 1, put 18.4g (0.8mol) sodium metal into a 250ml four-necked bottle equipped with electric stirring, a thermometer and a condenser, and slowly add 11.6g (0.1mol) pentapentyl A mixture of methyl ester, 96g methanol and 19.5g octanol, after the dropwise addition, slowly raise the temperature to 75-80°C, react for 1-2 hours, and then precipitate under normal pressure to remove excess methanol. Then slowly add 100ml of water, rectify the reaction solution, collect methanol solution at 63-65°C (after treatment for the next batch of feeding), and collect 6.9 grams of neopentyl alcohol at 113-114°C, with a yield of 80%. The purity of the product is 99.93%.

[0018] Example 2, put 13.8g (0.6mol) sodium metal into a 250ml four-necked bottle equipped with electric stirring, thermometer and condenser, slowly add 13g (0.1mol) ethyl pivalate dropwise into the bottle at room temperature The mixture of ester, 106g ethanol and 26g octanol is slowly heated to 75-80°C after the d...

Embodiment 4

[0020] Embodiment 4, 374kg sodium metal is dropped into in the reaction kettle of 5000 liters that is equipped with electric stirring, thermometer and condenser, in bottle, slowly drip the mixture of 236kg methyl pivalate and 407kg methyl alcohol and 400kg ethylene glycol under normal temperature After the dropwise addition, the temperature of the mixture was slowly raised to 75-80°C, and after 5 hours of reaction, 1546 kg of methanol was added dropwise, and the mixture was reacted for 3 hours. Then desolventize under normal pressure to remove excess methanol. Then slowly add 1500kg of water, distill the reaction liquid, collect the methanol solution at 63-65°C (after treatment, it will be used for the next batch of feeding), the reaction liquid is layered, take the organic phase, rectify, and collect the fresh water at 113-114°C Pentanol product 245kg, yield 79.3%, the purity of product is greater than 99.94%.

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Abstract

The invention discloses a new synthetic method for preparing high-content neopentyl alcohol. The method is as follows: with solvent A and alcohol medium at 50-90 DEG C, reduction reaction is carried out between esters of pivalic acid and metallic sodium. R is methyl or ethyl. After the solvent is removed from the generated sodium alkoxide, the sodium alkoxide is hydrolyzed and rectified for obtaining a neopentyl alcohol product with high purity, and the invention is characterized in that the product purity is higher than 99.9%.

Description

technical field [0001] The invention relates to a synthesis method for preparing high-content neopentyl alcohol by using the general formula I. [0002] [0003] [0004] Formula Ⅰ [0005] where R 1 is methyl or ethyl. [0006] The method includes the following steps: [0007] Metal sodium reacts with the raw material of general formula I, solvent A and the mixed solution of alcohol at a certain temperature, then distills off excess alcohol under reduced pressure, then acidifies with water and rectifies to obtain high-content neopentyl alcohol. Background technique [0008] Neopentyl alcohol is an important organic compound widely used in the production of pesticides, medicines or electrochemical products. Its preparation method has long been known to everyone. In summary, there are three main methods 1: Reduction of pivalic acid and its derivatives , including pivalic acid, methyl or ethyl pivalate, pivaloyl chloride and pivalamide were reduced with lithium aluminu...

Claims

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Application Information

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IPC IPC(8): C07C31/125C07C29/00C07C29/147
CPCC07C29/147C07C31/125
Inventor 不公告发明人
Owner ZHANGJIAKOU SIRUIKAI TECH