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Synthesis of 4,5-dimethyl-1,3-dioxane amylene-2-one

A dioxole, chemical synthesis technology, applied in 4, can solve diphosgene refining difficulties, storage and transportation difficulties, safety hazards and other problems, to achieve great implementation value and social and economic benefits, low production cost, production Safe and reliable effect

Inactive Publication Date: 2005-02-23
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because phosgene is a highly toxic gas that is strictly controlled and restricted internationally, there are great safety hazards in the use of phosgene in laboratories or industrial production
Diphosgene is a liquid. Although its safety is much greater than that of phosgene, it is easy to decompose when heated, especially when it encounters organic amines, activated carbon, ash, etc., and it is difficult to refine diphosgene. Storage and Transportation is also difficult, and there are still major safety hazards in the process of use

Method used

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  • Synthesis of 4,5-dimethyl-1,3-dioxane amylene-2-one

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] The molar ratio of feeding is: 3-hydroxy-2-butanone:bis(trichloromethyl)carbonate:auxiliary agent=1:0.33:1.0; the auxiliary agent is N-methylpyrrole. The organic solvent is carbon tetrachloride, and its consumption is 8 times of the quality of 3-hydroxyl-2-butanone;

[0010] Add 44g of 3-hydroxy-2-butanone, additives and organic solvents into a 500ml four-neck flask equipped with mechanical stirring, a constant pressure dropping funnel, a reflux condenser, and a thermometer. Under stirring, cool to 0°C, and then drop Add an organic solvent solution of bis(trichloromethyl)carbonate, and stir the reaction at 0-5°C for 2-3 hours. After the organic solvent is recovered by distillation under reduced pressure, an oily liquid is obtained, and then the temperature is slowly raised to 160°C. Stir at -165°C for 60 minutes, cool to below 25°C, add 160ml of water and 300ml of ether, stir for 15 minutes to separate the layers, extract the water layer with an appropriate amount of et...

Embodiment 2

[0012] The molar ratio of feeding is: 3-hydroxy-2-butanone:bis(trichloromethyl)carbonate:auxiliary agent=1:0.33:1.0; the auxiliary agent is N-methylpyrrole. The organic solvent is carbon tetrachloride, and its consumption is 8 times of the quality of 3-hydroxyl-2-butanone;

[0013] Under the protection of nitrogen, 3-hydroxy-2-butanone (44g), additives and organic solvents were successively added to a 500ml four-neck flask equipped with mechanical stirring, constant pressure dropping funnel, reflux condenser and thermometer, and opened Stir and cool to 0°C under stirring, then add bis(trichloromethyl)carbonate organic solvent solution dropwise at 0-5°C. After the addition, continue to stir and react at 0-5°C for 2 hours, distill under reduced pressure to recover the organic solvent, then slowly heat the obtained oily liquid, and stir at 165-170°C for 60 minutes, cool to below 25°C, add 160ml of water and 300ml of diethyl ether, stirred for 15 minutes to separate the layers, t...

Embodiment 3

[0015] The molar ratio of feeding is: 3-hydroxy-2-butanone:bis(trichloromethyl)carbonate:auxiliary agent=1:0.35:1.1; the auxiliary agent is N-methylpyrrole. The organic solvent is carbon tetrachloride, and its consumption is 10 times of the quality of 3-hydroxyl-2-butanone;

[0016] Under the protection of nitrogen, 3-hydroxy-2-butanone (44g), additives and organic solvents were successively added to a 500ml four-neck flask equipped with mechanical stirring, constant pressure dropping funnel, reflux condenser and thermometer, and opened Stir and cool to 0°C under stirring, then add bis(trichloromethyl)carbonate organic solvent solution dropwise at 0-5°C. After the addition, continue to stir and react at 0-2°C for 2 hours, recover the organic solvent by distillation under reduced pressure, then slowly heat the obtained oily liquid, and stir at 150-160°C for 75 minutes, cool to below 25°C, add 160ml of water and 300ml of diethyl ether, stirred for 15 minutes to separate the lay...

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Abstract

A process for chemically synthesizing 4,5-dimethyl-1,3-dioxyhetero pentene-2-one features that under the existance of proper assistant, the bis(trichloromethyl) sulfonate directly reacts on 3-hydroxy-2-butanone in organic solvent to obtain said product.

Description

technical field [0001] The invention relates to a method for preparing 4,5-dimethyl-1,3-dioxol-2-one by substituting bis(trichloromethyl)carbonate for phosgene and 3-hydroxy-2-butanone chemical synthesis method. 4,5-Dimethyl-1,3-dioxol-2-one is mainly used in the synthesis of new semi-synthetic antibiotics, such as the synthesis of semi-synthetic penicillin—Lenampicillin Hydrochloride Background technique [0002] Before the present invention is made, the existing main method of chemically synthesizing 4,5-dimethyl-1,3-dioxol-2-one is to be starting material with 3-hydroxyl-2-butanone and Produced by phosgene or diphosgene ring closure reaction, such as Tetrahedron Letters, 1972, 170-1704, USP 4428806, JP 6010571, US 4448732, etc. Because phosgene is a highly toxic gas that is strictly controlled and restricted in the world, there is a great potential safety hazard in the use of phosgene in laboratories or industrial production. Diphosgene is a liquid. Although its safety...

Claims

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Application Information

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IPC IPC(8): C07D317/38
Inventor 苏为科谢媛媛梁现蕊李永曙吴春雷施缃君
Owner ZHEJIANG UNIV OF TECH
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