Process for preparing 3, 3-dimethyl -2-pentanone

A technology for the reaction of dimethyl and dimethyl butyryl chloride is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of poor safety, difficult separation of by-products and products close to boiling points, and expensive raw materials. And other issues

Inactive Publication Date: 2006-06-07
LYNCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are four deficiencies in this method: 1. The process is more complicated and industrialization is more difficult; 2. The raw materials are more expensive; 3. The safety is poor; lower

Method used

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  • Process for preparing 3, 3-dimethyl -2-pentanone
  • Process for preparing 3, 3-dimethyl -2-pentanone
  • Process for preparing 3, 3-dimethyl -2-pentanone

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preparation example Construction

[0022] Raw material preparation

[0023] (1) Preparation of 2,2-dimethylbutyryl chloride

[0024] Under stirring, add 25.6g of 2,2-dimethylbutyric acid and 35.8g of thionyl chloride into the three-necked flask, heat to reflux, and absorb the generated hydrogen chloride and sulfur dioxide gas with lye. After no gas was produced, excess thionyl chloride was distilled off, and then distilled under reduced pressure to obtain 26.9 g of 2,2-dimethylbutyryl chloride, with a yield of 90%.

[0025] (2) Preparation of Diethyl Malonate Ethoxymagnesium

[0026] Under stirring, add 4g of absolute ethanol, 5.4g of magnesium powder, and then 0.5mL of carbon tetrachloride into the three-necked flask, and start the reaction after 3-5 minutes, and heat it slightly if necessary. After the reaction moderated, 150 mL of benzene was slowly added, and the reaction was kept boiling. Under stirring, a mixed solution of 35.2 g of diethyl malonate, 20 mL of absolute ethanol and 25 mL of benzene was ...

Embodiment 1

[0028] (1) 2, the preparation of 2-dimethyl butyryl malonate diethyl ester

[0029] Under stirring, a mixed solution of 26.9g of 2,2-dimethylbutyryl chloride and 50mL of benzene was added dropwise to the diethyl malonate ethoxymagnesium solution prepared above, and the dropwise addition was completed after about 15 minutes. Continue to stir and heat to reflux for about 1h. After the reaction solution was cooled, 220 mL of 10% sulfuric acid was added for acidification. The organic layer was separated, the aqueous layer was extracted once with 75 mL of benzene, and combined with the organic layer. The organic layer was washed with water, and benzene was recovered by distillation to obtain diethyl 2,2-dimethylbutyrylmalonate, which was used in the next reaction.

[0030] (2) Preparation of 3,3-dimethyl-2-pentanone

[0031] Under stirring, add 40mL of water, 14g of concentrated sulfuric acid, 60mL of acetic acid and the diethyl 2,2-dimethylbutyrylmalonate obtained from the abov...

Embodiment 2

[0035] Using tetrahydrofuran instead of benzene as the solvent, the preparation of the starting material and the step (1) of Example 1 were repeated. The reaction conditions of the step (2) of Example 2 are the same as those of the step (2) of Example 1, and finally 3,3-dimethyl-2-pentanone is obtained with a content of 98.6% and a yield of 81%. The resulting product is determined by infrared spectroscopy and mass spectrometry, and the results are the same as above.

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Abstract

The present invention relates to a process of preparing 3, 3-dimethyil-2-pentanone. The preparation process includes the following steps: reaction of magnesium alkoxyl ethyl malonate and 2-dimethyl butyryl chloride to prepare 2, 2-dimethyl butyryl ethyl malonate; and converting 2, 2-dimethyl butyryl ethyl malonate into 3, 3-dimethyil-2-pentanone. The preparation process of the present invention adopts cheap and facile material, and is simple, suitable for industry use and high in reaction yield.

Description

technical field [0001] The invention relates to a method for preparing 3,3-dimethyl-2-pentanone, in particular to a method for preparing 3,3-dimethyl-2-pentanone by using 2,2-dimethylbutyric acid as a raw material Methods. Background technique [0002] 3,3-Dimethyl-2-pentanone is an important pharmaceutical intermediate and pesticide intermediate, which is used in the synthesis of antibacterial agent-triazinyl(phenyl)propenol and insecticide 1-carbamoyl imidazole. At present, there are few reports about the synthesis of 3,3-dimethyl-2-pentanone, and the usual method is to use tert-amyl alcohol as raw material disclosed in J.Amer.Chem.Soc., 1976,6699-7007. Preparation. The method comprises the following steps: preparing tert-pentyl chloride by chlorination of tert-amyl alcohol; reacting tert-pentyl chloride with magnesium metal to prepare tert-amyl magnesium chloride; reacting tert-amyl magnesium chloride with acetyl chloride to prepare 3,3-dimethyl -2-Pentanone. There ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/04C07C45/00C07C45/61
Inventor 赵晨阳付立民
Owner LYNCHEM
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