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Preparation method of 3,3-methyl butyraldehyde

A technology of dimethylbutyraldehyde and dimethylbutyric acid, which is applied in 3 fields, can solve the problems of difficult acquisition and preservation of raw materials, difficulty in controlling the reaction process, waste of materials and energy, etc., and achieves easy acquisition, preservation, and reaction process Easy, low-cost preparation effects

Active Publication Date: 2011-11-16
陕西天汉生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, there are many methods for preparing 3,3-dimethylbutyraldehyde, and they all have certain defects: the raw materials are not easy to obtain and store, the reaction mechanism is relatively complicated, and high temperature and high pressure conditions are required, so there is certain danger. The process is difficult to control, and it is easy to produce by-products, resulting in waste of materials and energy. In addition, high temperature and high pressure conditions also lead to high preparation costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Follow the steps below to prepare 3,3-dimethylbutyraldehyde:

[0020] (1) Reaction to generate ester: first put in 1 part of 3,3-dimethylbutyric acid, 1.11 parts of ethanol, and 0.005 parts of sulfuric acid, heat up to 80°C and reflux for 2 hours, let stand to separate the lower layer of concentrated sulfuric acid after cooling, and then replenish Add 0.005 parts of concentrated sulfuric acid and 0.15 parts of ethanol, and then reflux for 3 hours, then stand for stratification, separate the lower layer of concentrated sulfuric acid, heat up to the temperature of the kettle after stratification, distill off excess ethanol, and distill under reduced pressure to 115°C to obtain 3,3-Dimethyl butyric acid ethyl ester, the vacuum degree during vacuum distillation is -0.08Mpa, wherein the concentration of 3,3-dimethyl butyric acid is not less than 99%, the concentration of ethanol is not less than 95%, concentrated The concentration of sulfuric acid is not less than 98%, 3,3-d...

Embodiment 2

[0025] Follow the steps below to prepare 3,3-dimethylbutyraldehyde:

[0026] (1) Reaction to generate ester: first put in 1 part of 3,3-dimethylbutyric acid, 1.14 parts of ethanol, and 0.009 part of sulfuric acid, heat up to 80°C and reflux for 2 hours, let stand to separate the lower layer of concentrated sulfuric acid after cooling, and then add Add 0.005 parts of concentrated sulfuric acid and 0.35 parts of ethanol, and then reflux for 3 hours, then let it stand for stratification, separate the lower layer of concentrated sulfuric acid, heat up to 120°C after layering, distill off excess ethanol, and distill under reduced pressure to 115°C to obtain Ethyl 3,3-dimethylbutyrate, the vacuum degree during vacuum distillation is -0.09Mpa, the concentration of 3,3-dimethylbutyric acid is not less than 99%, the concentration of ethanol is not less than 95%, concentrated The concentration of sulfuric acid is not less than 98%, 3,3-dimethylbutyric acid and ethanol are used as raw ma...

Embodiment 3

[0031] Follow the steps below to prepare 3,3-dimethylbutyraldehyde:

[0032] (1) Reaction to generate ester: first put in 1 part of 3,3-dimethylbutyric acid, 1.12 parts of ethanol, and 0.006 parts of sulfuric acid, heat up to 80°C and reflux for 2 hours, let stand to separate the lower layer of concentrated sulfuric acid after cooling, and then add Add 0.006 parts of concentrated sulfuric acid and 0.2 parts of ethanol, and then reflux for 3 hours, then stand for stratification, separate the lower layer of concentrated sulfuric acid, heat up to the temperature of the kettle after layering, distill off excess ethanol, and distill under reduced pressure to 115°C to obtain Ethyl 3,3-dimethylbutyrate, the vacuum degree during vacuum distillation is -0.085Mpa, the concentration of 3,3-dimethylbutyric acid is not less than 99%, the concentration of ethanol is not less than 95%, concentrated The concentration of sulfuric acid is not less than 98%, 3,3-dimethylbutyric acid and ethanol ...

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Abstract

The invention discloses a preparation method of 3,3-methyl butyraldehyde, which comprises the following steps: (1) reacting to generating ester: putting 3,3-dimethyl butyric acid, ethanol and concentrated sulfuric acid into an enamel still for reacting, separating concentrated sulfuric acid at the lower layer after finishing the reaction, then performing a decompression distillation; (2) reacting to generating alcohol: putting tetrahydrofuran, potassium borohydride, anhydrous lithium chloride and anhydrous aluminium chloride, heating and dropping 3,3-dimethyl ethyl butyrate, refluxing, cooling and stirring by adding water, distilling once again; (3) reacting to generating aldehyde: putting dichloromethane, water, potassium bromide and 3,3-dimethylbutyrate, cooling, then dropping sodium hypochlorite and water, separating a crude 3,3-methyl butyraldehyde solution at the lower layer; (4) purifying aldehyde: putting water and sodium bisulfite into the enamel still, putting the crude 3,3-dimethylutyraldehyde solution, dichloromethane extract and sodium bicarbonate after stirring and dissolving, distilling to obtain the product. The invention has the advantages of simple reaction mechanism, easy control, easy raw material acquisition and low preparation cost.

Description

technical field [0001] The invention relates to a preparation method of 3,3-dimethylbutyraldehyde. Background technique [0002] At present, there are many methods for preparing 3,3-dimethylbutyraldehyde, and they all have certain defects: the raw materials are not easy to obtain and store, the reaction mechanism is relatively complicated, and high temperature and high pressure conditions are required, so there is certain danger. The process is difficult to control, and by-products are likely to be produced, resulting in waste of materials and energy. In addition, the high temperature and high pressure conditions also lead to high preparation costs, so it is not necessary to expand the production scale. Contents of the invention [0003] The purpose of the present invention is to provide a preparation method of 3,3-dimethylbutyraldehyde, which has mild reaction conditions, low preparation cost and is relatively safe. [0004] The object of the present invention is achieve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/02C07C45/30
Inventor 许峰
Owner 陕西天汉生物科技有限公司
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