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Synthesis method of full halogenated miscellaneous naphthene

A technology of heterocycloalkane and synthesis method, which is applied in the field of synthesis of perhalogenated heterocycloalkane, and can solve problems such as high reaction temperature and harsh reaction conditions

Inactive Publication Date: 2018-11-23
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solve the problems of high reaction temperature, harsh reaction conditions, and incompletely halogenated hydrogen-containing halogenated heterocycloalkanes in the technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 1000ml four-neck flask with mechanical stirring and a reflux condenser, add 329g (1.0mol) of 1-bromo-2,2-diacetoxypentafluoropropane, 280g (2.0mol) of difluoromalonic acid, 10g of para Toluenesulfonic acid, stirred, heated to 120 ° C, regularly sampled and analyzed, when it was detected that the reaction was over, cooled, and 272g of 2-trifluoromethyl-2-difluorobromomethyl-4,6-dioxo-5 was isolated -Difluoro-1,3-dioxane, yield 78%.

[0024] In a 1000ml pressure reactor, add 175g (0.5mol) of the above-prepared 2-trifluoromethyl-2-difluorobromomethyl-4,6-dioxo-5-difluoro-1,3-diox Heterocyclohexane, 300g dichloromethane, 324g sulfur tetrafluoride, stirred, and reacted at 120°C. After the reaction, cooled and separated to obtain 106g 2-trifluoromethyl-2-difluorobromomethyl-4 , 4,6,6-tetrafluoro-5-difluoro-1,3-dioxane, the yield was 54%, and the corresponding hydrogen-containing dioxane impurity was not detected.

Embodiment 2

[0026] In a 500ml four-neck flask with mechanical stirring and reflux condenser, add 268g (1.0mol) 2,2-diacetoxyhexafluoropropane, 108g oxalic acid (1.2mol), 5g concentrated sulfuric acid, stir, and heat up to 140°C , regular sampling analysis, when it is detected that the reaction is over, it is cooled to separate 201.5g2,2-bis(trifluoromethyl)-4,5-dioxo-1,3-dioxolane, yield 84.7%.

[0027]In a 1000ml four-neck flask with mechanical stirring and a reflux condenser, add 312g (1.5mol) of phosphorus pentachloride, 500g of phosphorus oxychloride and 119g (0.5mol) of the 2,2-bis(trifluoromethyl) prepared above )-4,5-dioxo-1,3-dioxolane, stirred, heated to 100°C, and reacted at 100°C. After the reaction, 142g of 2,2-bis(trifluoromethyl)-4,4,5,5-tetrachloro-1,3-dioxolane was separated by cooling, the yield was 81.6%, and no corresponding Hydrogen-containing dioxolane impurity.

Embodiment 3

[0029] In a 1000ml four-neck flask with mechanical stirring and reflux condenser, add 301g (1.0mol) 1,3-dichloro-2,2-diacetoxytetrafluoropropane, 180g (2mol) oxalic acid, 30g trichloride Iron, 300g of 1-ethyl-3-methylimidazolium tetrafluoroborate, stirred, heated up to 50°C, regularly sampled and analyzed, when it was detected that the reaction was over, cooled, and 250.7g of 2,2-bis(difluorochloro Methyl)-4,5-dioxo-1,3-dioxolane, yield 92.5%.

[0030] In a 1000ml four-neck flask with mechanical stirring and a reflux condenser, add 136g (0.5mol) of 2,2-bis(difluorochloromethyl)-4,5-dioxo-1,3- Dioxolane, 100g DMF, stirred, heated up to 70°C, 357g (3.0mol) of thionyl chloride was added dropwise, and after the addition of thionyl chloride was completed, the reaction was carried out under reflux. After the reaction was completed, 85.5g of 2,2-bis(difluorochloromethyl)-4,4,5,5-tetrachloro-1,3-dioxolane was obtained by cooling and separation, with a yield of 45%, undetected Out of...

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Abstract

The invention discloses a synthesis method of full halogenated miscellaneous naphthene. According to the method, diacetyloxy halogenated alkanes and full halogenated diacid react to generate corresponding oxo miscellaneous naphthene; the oxo miscellaneous naphthene reacts with halogenating agents to generate target products of full halogenated miscellaneous naphthene. The reaction of the synthesismethod can be realized in an ordinary glass reaction vessel or a pressure reaction kettle; the product of the full halogenated miscellaneous naphthene does not contain hydrogen-containing halogenatedmiscellaneous naphthene which is not completely halogenated; the anti-corrosion and anti-aging performance of polymers can be improved. The problems of high reaction temperature, harsh reaction conditions, existence of hydrogen-containing halogenated miscellaneous naphthene which is not completely halogenated, and the like in the prior art are solved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for synthesizing perhalogenated heterocycloalkanes. Background technique [0002] Perhalogenated heterocycloalkanes, especially perfluorooxacycloalkanes containing dichloro(bromo, iodo) groups, can generate perfluorooxacycloalkenes through dehalogenation reaction. Perfluorooxoheterocyclic olefins are very important fluorine-containing monomers, which are used to prepare fluorine-containing amorphous homopolymers, and can also be combined with ethylene, propylene, tetrafluoroethylene, trifluoropropylene, trifluorochloroethylene, etc. Preparation of a new type of amorphous fluorine-containing copolymer by bulk copolymerization. This new type of fluoroplastic has low refractive index and low dielectric constant, good light transmission, and excellent corrosion and aging resistance, and can be used as insulating encapsulation material for optical cable...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/06C07D317/42
Inventor 叶立峰张坚文
Owner JUHUA GROUP TECH CENT