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Synthesis method of oxetanone

A technology of oxetanone and a synthesis method, applied in the formation/introduction of carbonyl group, organic chemistry and other directions, can solve the problems of less 3-oxetanone, hidden danger, high price and the like, and achieves improved reaction yield , the effect of reducing production costs and cheap materials

Active Publication Date: 2014-04-02
赣州康瑞泰药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] Although these methods can all produce 3-oxetanone, there are unavoidable potential safety hazards in the enlarged production, or can not meet environmental protection requirements, so that there are very few manufacturers producing 3-oxetanone, and its price Extremely expensive, which seriously hinders its further application and development in organic chemistry and biomedicine

Method used

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  • Synthesis method of oxetanone
  • Synthesis method of oxetanone
  • Synthesis method of oxetanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048]Add 3 L of dichloromethane, 1.24 kg of TCCA, 1.28 kg of sodium bicarbonate, 33 g of potassium bromide and 8.7 g of TEMPO into a 5 L dry three-necked flask, stir and cool down to -5°C under nitrogen protection. Then 400 g of oxetanone was added dropwise. After the dropwise addition was complete, stirring was continued at 0°C for 2 hours. After filtering the reaction mixture, it was distilled under reduced pressure at room temperature to obtain 350 g of the product (purity greater than 95%), and the yield was 89%.

Embodiment 2

[0050] Add 2.0 L of dichloromethane, 770 kg of NCS, 710 kg of potassium bicarbonate, 150 g of tetrabutylammonium bromide and 15 g of TEMPO into a 5 L dry three-necked flask, stir and cool down to -5°C under nitrogen protection. Then 400 g of oxetanone was added dropwise. After the dropwise addition was complete, stirring was continued at 25°C for 4 hours. After the reaction mixture was filtered, it was distilled under reduced pressure at room temperature to obtain 320 g of the product (purity greater than 95%), with a yield of 82%.

Embodiment 3

[0052] Add 2.5 L of dichloromethane, 1.92 kg of NBS, 1.48 kg of potassium carbonate, 25 g of sodium bromide and 25 g of TEMPO into a 5 L dry three-necked flask, stir and cool down to 0 °C under nitrogen protection. Then 400 g of oxetanone was added dropwise. After the dropwise addition was complete, stirring was continued at 25°C for 4 hours. After the reaction mixture was filtered, it was distilled under reduced pressure at room temperature to obtain 335 g of the product (purity greater than 95%), with a yield of 86%.

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Abstract

The invention discloses a synthesis method of oxetanone. The method comprises the steps: in an organic solvent and in the presence of a catalyst, a halide and an alkali, utilizing an oxidant to oxidize oxetanol, and then separating and purifying to obtain oxetanone. The method adopts the organic oxidation system for oxidation production of oxetanone for the first time, is cheap in adopted materials and simple in operation, avoids use of methyl azide, butyl lithium, or 1,3-dichloroacetone and other dangerous chemicals, enables the synthesis method of oxetanone to be safely amplified, and can be produced in large scale; the method is friendly to the environment and avoids use of phosphorus pentoxide and other reagents, so that the process meets the requirements of environmental protection; and moreover, the method increases the reaction yield which is increased from 50% to 80% or more, thereby greatly reducing the production cost, and being in favor of further application and development of oxetanone in organic chemistry and biological medicines.

Description

Technical field [0001] The present invention involves a synthesis method for a hydrocet ketone. Background technique [0002] In the research and development of small molecules of drugs, because some positions of the small molecules of drugs are easily degraded by biology, the activity is lost. Usually, a double -substituted methyl group is introduced in these positions to avoid the active drug small molecules from being degraded by biology.However, the introduction of double -replacement methyl -based methyls will greatly increase the lipidity of drug activity molecules, which may make the small molecules of the drug more likely to be metabolized.Therefore, looking for a more stable small base that does not change its lipophytic to replace the dual -replacement methyl group has become a very important and urgent goal for the drug small molecules.Eric Carreira and others have found that the introduction of 3-oxygen methane on the small molecules of drugs can reduce its lipidabili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/10C07B41/06
CPCC07D305/10
Inventor 龙翔天王勇郎丰睿
Owner 赣州康瑞泰药业有限公司
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