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Method for synthesizing 3,3-dimethyl butyraldehyde

A technology of dimethylbutyraldehyde and compounds, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carbonyl compounds by hydrolysis, etc., can solve the problems of complex post-treatment, large waste water generation, expensive raw materials, etc., and achieve the improvement of crude products and The effect of finished product yield, reduction of reaction impurities, and simple operation

Pending Publication Date: 2018-11-13
NANTONG CHANGHAI FOOD ADDITIVE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of the prior art 3,3-dimethylbutyraldehyde synthesis method, such as expensive raw materials, complicated post-treatment, and more waste water, and provide a simple process, convenient operation, cost saving, and environmental protection. Safe Synthesis of 3,3-Dimethylbutyraldehyde

Method used

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  • Method for synthesizing 3,3-dimethyl butyraldehyde
  • Method for synthesizing 3,3-dimethyl butyraldehyde
  • Method for synthesizing 3,3-dimethyl butyraldehyde

Examples

Experimental program
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Embodiment 1

[0026] In a 2000ml four-neck flask, put into 400.0g of dichloromethane and 20.0g of solid AlCl after the thermometer is fully replaced with nitrogen. 3 / Al 2 o 3 , cooled to -10°C, then slowly added 203.6g of tert-butyl chloride (2.2mol) dropwise, and the dropwise addition was completed within 1 hour, then began to dropwise add 200g of vinyl propionate (2mol), within 1 hour after the dropwise addition was completed, keep the temperature After reacting for 2 hours, the catalyst was removed by filtration, and the catalyst was recovered. Then the organic layer was distilled under reduced pressure to remove low boiling point substances to obtain an intermediate, 700g NaOH (15%) aqueous solution was added to the intermediate, heated to 110°C for reflux and hydrolyzed for 10 hours to obtain the crude product 3,3-dimethylbutyraldehyde , the crude product was rectified to obtain 3,3-dimethylbutyraldehyde with a purity of 99.0%, and a yield of 80%.

Embodiment 2

[0028] In a 2000ml four-necked flask, put into 400.0g of dichloroethane and 59.0g of solid TiO after the thermometer is fully replaced with nitrogen. 2 / SO 4 2- , cooled to -8°C, then slowly added 185.1g of tert-butyl chloride (2mol) dropwise, and the dropwise addition was completed within 1 hour, and then began to dropwise add 258.3g of vinyl acetate (3mol), and after the dropwise addition was completed within 1 hour, the insulation reaction After 2 hours, the catalyst was removed by filtration, and the catalyst was recovered. Then the organic layer was distilled under reduced pressure to remove low-boiling substances to obtain an intermediate, and 2.0 g of catalyst amberlyst35 and 200.0 g of deionized water were added to the intermediate, heated to 90° C., refluxed and hydrolyzed for 2 hours. After the catalyst was filtered, the crude product 3,3- Dimethylbutyraldehyde, the crude product is rectified to obtain 3,3-dimethylbutanal with a purity of 99.1%, and the yield is 83...

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Abstract

The invention provides a technological method for synthesizing 3,3-dimethyl butyraldehyde. The technological method comprises the following steps: adding an organic solvent and a solid acid catalyst into a container under the protection of nitrogen gas; dropwise adding tert-butyl chloride; then dropwise adding alkyl acid type vinyl ester; carrying out heat-insulation reaction, then filtering to remove a catalyst; then decompressing and distilling an organic layer; then adding alkali or acid, and heating, refluxing and hydrolyzing to obtain a crude product; then rectifying the crude product toobtain a 3,3-dimethyl butyraldehyde finished product. The technological method has the advantages of low raw material cost, mild reaction conditions, simplicity in operation and few side reaction, safety and environmental protection, and industrialized production is facilitated.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for synthesizing 3,3-dimethylbutyraldehyde. Background technique [0002] Neotame is a new type of non-nutritive high-efficiency sweetener, developed by Newtrathwaite, its chemical name is N-[N-3,3-dimethylbutyl]-L-ɑ- Aspartame]-L-phenylalanine 1-methyl ester has the advantages of high sweetness, low calorie, good stability, etc. It is safe and harmless to human body and has huge market potential, while 3,3-dimethyl Butyraldehyde is an important intermediate of neotame. Due to the limited market quantity, it is expensive, so a new synthetic method needs to be studied. [0003] At present, the existing disclosed methods for synthesizing 3,3-dimethylbutyraldehyde include: in the patent US6573409, isobutylene and ethylene are used as raw materials to prepare 3,3-dimethylbutyraldehyde through the acid hydration oxidation method, which requires equipment High, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/42C07C47/02
CPCC07C45/42C07C67/293C07C47/02C07C69/63
Inventor 庄勇王立平赵海东顾京城
Owner NANTONG CHANGHAI FOOD ADDITIVE
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