Preparation method of 3,9-difluoro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane

The technology of a diphosphorus spiro ring and a synthesis method is applied in the field of preparation of a fluorine-containing bisphosphorus spiro ring compound, which can solve the problems of lowering the purity and the like, and achieve the effects of simple operation and low price.

Pending Publication Date: 2020-07-03
浦拉司科技(上海)有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no report on the synthesis of 3,9-difluoro-2,4,8,10-tetraoxo-3,9-diphosphospiro[5.5]undecane. Reactive reaction and hydrolysis, thereby reducing the purity

Method used

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  • Preparation method of 3,9-difluoro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane
  • Preparation method of 3,9-difluoro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane
  • Preparation method of 3,9-difluoro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022]

[0023] A) Stir and mix pentaerythritol (136.2g, 1mol), phosphorus trichloride (302.1g, 2.2mol) and toluene (276.4g, 3mol), cool down to about 10°C, add pyridine (1.36g) dropwise, and drop to 10°C Stir left and right for 30 minutes, slowly raise the temperature to 50°C and react for 3 hours, hydrogen chloride will be generated, and it should be absorbed well. Sampling and GC detection of raw materials < 2%, after the reaction is over, phosphorus trichloride and toluene are recovered by vacuum distillation, and the intermediate product 3,9-dichloro-2,4,8,10-tetraoxo-3,9-di Phosphorus spiro[5.5]undecane 251.7g, GC 92.5%, yield 95%.

[0024] B) The above-mentioned intermediate 3,9-dichloro-2,4,8,10-tetraoxo-3,9-diphosphospiro[5.5]undecane (251.7g, 0.95mol) and toluene (500g) Stir and cool down to 0°C, then add antimony trifluoride (126.9g, 0.71mol) in batches, stir for 1 hour after adding at about 0°C, then slowly raise the temperature to 20°C for 10-20 hours, sample ...

Embodiment 2

[0026]

[0027] A) Pentaerythritol (136.2g, 1mol), phosphorus trichloride (302.1g, 2.2mol) and toluene (276.4g, 3mol) were stirred and mixed, cooled to about 10°C, and 4-methylpyridine (2.2g) was added dropwise, Stir at about 10°C for 30 minutes after dropping, slowly raise the temperature to 55°C and react for 3 hours, nitrogen bubbles during the heating reaction process, blow out the hydrogen chloride produced by the reaction, and absorb the hydrogen chloride with sodium hydroxide aqueous solution. Sampling and GC detection of raw materials < 2%, after the reaction is over, phosphorus trichloride and toluene are recovered by vacuum distillation, and the intermediate product 3,9-dichloro-2,4,8,10-tetraoxo-3,9-di Phosphorus spiro[5.5]undecane 249.6g, GC 93.1%, yield 94.2%.

[0028] B) The above-mentioned intermediate 3,9-dichloro-2,4,8,10-tetraoxo-3,9-diphosphospiro[5.5]undecane (249.6g, 0.942mol) and dichloromethane ( 500g) stirring and cooling down to 0°C, dropwise addin...

Embodiment 3

[0030]

[0031] A) Stir and mix pentaerythritol (136.2g, 1mol), phosphorus tribromide (568.5g, 2.1mol), toluene (276.4g, 3mol), cool down to about 10°C, add pyridine (1.36g) dropwise, and drop to 10°C Stir left and right for 30 minutes, slowly raise the temperature to 45°C and react for 4 hours. During the heating reaction process, nitrogen bubbles are blown out to blow out the hydrogen bromide produced by the reaction, and the hydrogen bromide is absorbed with sodium hydroxide aqueous solution. Sampling and GC detection of raw materials < 2%, after the reaction is over, phosphorus tribromide and toluene are recovered by vacuum distillation, and the intermediate product 3,9-dibromo-2,4,8,10-tetraoxo-3,9-distilled is obtained by distillation Phosphorus spiro[5.5]undecane 339.4g, GC 91.9%, yield 95.9%.

[0032] B) The above-mentioned intermediate 3,9-dichloro-2,4,8,10-tetraoxo-3,9-diphosphospiro[5.5]undecane (339.4g, 0.959mol) and dichloromethane ( 750g) was stirred and cool...

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Abstract

The invention discloses a preparation method of 3,9-difluoro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane, belonging to the field of organic synthesis. The preparation method comprises the following steps: carrying out a heating reaction on pentaerythritol and phosphorus trihalide in the presence of a catalyst, and carrying out distilling to obtain an intermediate 3,9-dihalogeno-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane; reacting the intermediate with a fluorination reagent, and carrying out cooling and filtering after the reaction; and carrying out reduced-pressure distillation to obtain the 3,9-difluoro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane. The raw materials used in the method are low in price, and the method is simple and convenient to operate and suitable forindustrial production.

Description

technical field [0001] The present invention relates to a preparation method of a fluorine-containing diphosphorous spirocyclic compound, in particular to a 3,9-difluoro-2,4,8,10-tetraoxo-3,9-diphosphorous spiro[5.5]deca Improved preparation of monoalkanes. Background technique [0002] 3,9-difluoro-2,4,8,10-tetraoxo-3,9-diphosphospiro[5.5]undecane is an important electronic chemical, and its special structure can be used in lithium electronics Electrolyte additive. [0003] At present, there is no report on the synthesis of 3,9-difluoro-2,4,8,10-tetraoxo-3,9-diphosphospiro[5.5]undecane. Reactive reaction and hydrolysis, thereby reducing the purity. [0004] Therefore, it is extremely necessary to develop a synthetic process method with easy-to-obtain raw materials, environmentally friendly solvents, and suitable for industrial production. Contents of the invention [0005] In order to solve the above technical problems, the present invention provides a preparation met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6571
CPCC07F9/6571
Inventor 蔡伟兵漆伟君
Owner 浦拉司科技(上海)有限责任公司
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