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Preparation method for 3,3-dimethylbutyraldehyde

A technology of dimethyl butyraldehyde and dimethyl butanol, which is applied in the field of preparation of 3,3-dimethyl butyraldehyde, can solve the problems of violent exothermic reaction, difficult control of large-scale production, low product purity and the like

Inactive Publication Date: 2014-03-26
太仓浦源医药原料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The yield of this method is high, up to 80%, but the purity of the product obtained is low, and the reaction is violently exothermic, and it is difficult to control large-scale production

Method used

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  • Preparation method for 3,3-dimethylbutyraldehyde
  • Preparation method for 3,3-dimethylbutyraldehyde
  • Preparation method for 3,3-dimethylbutyraldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 51g (0.5mol) of 3,3-dimethylbutanol and 2,2,6,6-tetramethyl-1-piperidinyl oxygen radical and potassium bromide compound salt 9.8 into a 2000ml four-necked flask g (0.05mol), cooled to -10°C, and began to add 10% NaClO dropwise 2 Aqueous solution 1357ml (containing 1.5mol NaClO 2 ), keep the temperature between 0~-5°C during the dropping process, continue to stir after the dropping, slowly raise the temperature to 25°C for oxidation reaction, until the content of 3,3-dimethylbutanol is ≤1% when detected by GC Reaction finishes; after reaction finishes, add dichloromethane 300ml to extraction in reaction solution, then organic layer is washed with water, concentrated, vacuum distillation, obtains 40g of target product, and the content of 3,3-dimethylbutyraldehyde in target product is 98.5%, the yield is 80%.

Embodiment 2

[0039] Add 102g (1.0mol) of 3,3-dimethylbutanol, 500ml of THF and the compound of 2,2,6,6-tetramethyl-1-piperidinyloxy radical and potassium bromide into a 5000ml four-necked flask Salt 19.6g (0.1mol), cooled to -10°C, began to drop 10% NaClO by mass 2 2714ml aqueous solution (containing 3molNaClO 2 ), keep the temperature between 0~-5°C during the dropping process, continue to stir after the dropping, slowly raise the temperature to 25°C for oxidation reaction, until the content of 3,3-dimethylbutanol is ≤1% when detected by GC Reaction finishes; after reaction finishes, add dichloromethane 600ml to extraction in reaction liquid, then organic layer is washed with water, concentrates, decompression distillation, obtains 85g of target product, and the content of 3,3-dimethylbutyraldehyde in target product is 98.5%, the yield is 85%.

Embodiment 3

[0041] Add 102g (1.0mol) of 3,3-dimethylbutanol, 2,2,6,6-tetramethyl-1-piperidinyl oxygen radical and potassium bromide compound salt 19.6 into a 5000ml four-necked flask g (0.1mol) and 10g of butylammonium bromide, cooled to -10°C, and began to add dropwise NaClO with a mass percentage of 10%. 2 2714ml aqueous solution (containing 3molNaClO 2 ), keep the temperature between 0~-5°C during the dropping process, continue to stir after the dropping, slowly raise the temperature to 25°C for oxidation reaction, until the content of 3,3-dimethylbutanol is ≤1% when detected by GC The reaction is over; after the reaction is over, add 600ml of dichloromethane to the reaction solution for extraction, then wash the organic layer with water, concentrate, and distill under reduced pressure to obtain 87g of the target product, and the content of 3,3-dimethylbutyraldehyde in the target product is 98.6%, the yield is 87%.

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Abstract

The invention discloses a preparation method for 3,3-dimethylbutyraldehyde. According to the method, under the effect of a catalyst 2,2,6,6-tetramethyl-1-piperidinyloxy free radicals or salts thereof, 3,3-dimethyl-1-butanol and sodium chlorite are subjected to oxidation reaction, so that 3,3-dimethylbutyraldehyde is obtained. The product (3,3-dimethylbutyraldehyde) prepared through the method disclosed by the invention has the advantages that the purity is high, and can reach more than 98.5%, and the yield is high, and can reach more than 80%, and the preparation method is an ideal preparation method for 3,3-dimethylbutyraldehyde, and is suitable for scale production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 3,3-dimethylbutyraldehyde. Background technique [0002] Neotame is a new type of strong dipeptide sweetener, which is a derivative of aspartame. Its stability and use cost are better than aspartame. It has attracted the attention of the world's food industry since it came out. . In July 2002, FDA officially approved the use of neotame in food. China also approved the use of neotame in various foods in April 2003, and added it according to production needs. 3,3-Dimethylbutyraldehyde is an important intermediate in the synthesis of neotame, and its purity and cost directly affect the purity of sweetness and price of neotame. [0003] The existing methods for synthesizing 3,3-dimethylbutyraldehyde (DMBA) mainly include: [0004] Method 1: Hydration and oxidation of isobutylene ethylene acid (refer to Patent No. US6,573,409, the date of authoriz...

Claims

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Application Information

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IPC IPC(8): C07C45/30C07C47/02
CPCC07C45/30
Inventor 周富荣王俊邵林华
Owner 太仓浦源医药原料有限公司
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