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Preparation method of epoxy fluoropropane

A technology of epoxyfluoropropane and propanol, which is applied in the field of preparation of epoxyfluoropropane, can solve the problems of unavailable, expensive starting materials, unsuitable for industrial production, etc., and achieve less by-products, high conversion rate and selectivity , The safe and controllable effect of the preparation process

Pending Publication Date: 2021-12-10
JIANGSU SANMEI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2018, the ChemMedChem journal disclosed a method for synthesizing epifluorohydrin using glycidyl p-toluenesulfonate as the starting material. The starting material of this method is expensive and not easy to obtain, and can only be used as a small amount of synthesis in the laboratory. , not suitable for industrial production

Method used

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  • Preparation method of epoxy fluoropropane
  • Preparation method of epoxy fluoropropane

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Preparation of 1,3-dichloro-2-propanol

[0030] Add 500 g of glycerin and 25 g of acetic acid into a 1 L reaction flask equipped with a gas distributor, condensing reflux tube, and water separator, stir, and slowly raise the temperature to 110°C. Introduce hydrogen chloride gas at a rate of 0.1kg / h, start condensation, and separate water. Pass through hydrogen chloride gas for 4h, stop the reaction, and slowly cool down to room temperature. Aqueous sodium bicarbonate solution was added, and the layers were separated. Add 4 g of anhydrous calcium chloride to the organic layer, dry and filter to obtain 625 g of the product 1,3-dichloro-2-propanol with a yield of 89.1%.

[0031] (2) Preparation of 1,3-difluoro-2-propanol

[0032] Add 625g of 1,3-dichloro-2-propanol obtained above into a 2L reaction flask, add 500ml of propionamide and 420g of potassium fluoride, stir and heat up. Raise the temperature to 180°C, keep the temperature for 2 hours, stop the reaction, a...

Embodiment 2

[0036] (1) Preparation of 1,3-dichloro-2-propanol

[0037] Add 500 g of glycerin and 25 g of acetic acid into a 1 L reaction flask equipped with a gas distributor, condensing reflux tube, and water separator, stir, and slowly raise the temperature to 110°C. Introduce hydrogen chloride gas at a rate of 0.1kg / h, start condensation, and separate water. Pass through hydrogen chloride gas for 4h, stop the reaction, and slowly cool down to room temperature. Aqueous sodium bicarbonate solution was added, and the layers were separated. Add 4 g of anhydrous calcium chloride to the organic layer, dry and filter to obtain 625 g of the product 1,3-dichloro-2-propanol with a yield of 89.1%.

[0038] (2) Preparation of 1,3-difluoro-2-propanol

[0039] Add 625g of 1,3-dichloro-2-propanol obtained above into a 2L reaction flask, add 500ml of propionamide and 520g of potassium fluoride, stir and heat up. Raise the temperature to 180°C, keep the temperature for 2 hours, stop the reaction, a...

Embodiment 3

[0043] (1) Preparation of 1,3-dichloro-2-propanol

[0044] Add 500 g of glycerin and 40 g of adipic acid into a 1 L reaction flask equipped with a gas distributor, condensing reflux tube, and water separator, stir, and slowly raise the temperature to 120°C. Introduce hydrogen chloride gas at a rate of 0.1kg / h, start condensation, and separate water. Pass through hydrogen chloride gas for 4h, stop the reaction, and slowly cool down to room temperature. Aqueous sodium bicarbonate solution was added, and the layers were separated. 4 g of anhydrous calcium chloride was added to the organic layer, dried and filtered to obtain 642 g of the product 1,3-dichloro-2-propanol with a yield of 91.5%.

[0045] (2) Preparation of 1,3-difluoro-2-propanol

[0046] Add 642g of 1,3-dichloro-2-propanol obtained above into a 2L reaction flask, add 500ml of propionamide and 310g of sodium fluoride, stir and heat up. Raise the temperature to 180°C, keep the temperature for 2 hours, stop the reac...

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Abstract

The invention discloses a preparation method of epoxy fluoropropane, which comprises the following steps: (1) chlorination: by taking glycerol as an initial raw material and carboxylic acid as a catalyst, continuously introducing hydrogen chloride gas at 50-150 DEG C until the reaction is finished, stopping introducing hydrogen chloride, and carrying out post-treatment to obtain a product 1, 3-dichloro-2-propanol; (2) fluorine-chlorine exchange: adding propanamide into the obtained product 1, 3-dichloro-2-propanol, adding inorganic fluoride salt at the same time, heating to 150-250 DEG C, reacting for 1-5 hours, stopping the reaction, and separating to obtain 1, 3-difluoro-2-propanol; and (3) Williamson cyclization: adding the 1, 3-difluoro-2-propanol into a reaction kettle, adding a strong base and a dispersing solvent, reacting for 1-8 hours at the temperature of -20 to 50 DEG C, and after the reaction is finished, filtering and rectifying to obtain the product epoxy fluoropropane. The preparation method has the advantages of cheap and easily available raw materials, mild and controllable reaction process, greenness and economy, and is suitable for industrialization.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of epifluorohydrin. Background technique [0002] Fluorine is the most electronegative element among all the elements discovered so far. Its atomic radius is similar to that of hydrogen atoms. It has strong biological activity and pseudo-mimetic effect. More than 40% of new drugs in China are fluorine-containing varieties. In addition, due to the super stability of the C-F bond constructed with carbon atoms, fluorine-containing compounds have excellent physical and chemical properties, and are widely used in dyes, refrigerants, new materials and other fields, and are the strategic focus of my country's chemical industry development. New Direction. It is an effective method for developing new materials and a shortcut for developing new materials by using the characteristics of fluorine atoms to replace Cl or H in known compounds by imitation. For newly devel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/26
CPCC07D303/08C07D301/26
Inventor 赵恒军陈朝阳丛鑫鑫张伟郑爱伟
Owner JIANGSU SANMEI CHEM
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