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2-fluoropropionate synthetizing method

A technology of fluoropropionate and synthesis method, which is applied in the field of synthesis of 2-fluoropropionate, can solve the problems of high reaction temperature, low yield of potassium fluoride fluorination, high cost, etc., achieve mild reaction conditions and improve selectivity Sexuality and low cost effect

Active Publication Date: 2015-11-11
JUHUA GRP
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  • Abstract
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Problems solved by technology

[0003] The above-mentioned various methods for preparing 2-fluoropropionate all have certain weak points
The raw material cost of 2-chloropropionate is low, but the yield of fluorination with potassium fluoride is low, and the reaction temperature is high, resulting in a large amount of three wastes; fluorination with hydrogen fluoride is dangerous, the equipment is corroded seriously, and it is difficult to dispose of spent catalysts
The process route using 2-bromopropionate as raw material has high raw material price and high cost; the process route using 2-hydroxypropionate as raw material has the disadvantages of expensive fluorinated reagents and very dangerous operation.

Method used

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preparation example Construction

[0021] The invention provides a kind of synthetic method of 2-fluoro propionate, comprises the steps:

[0022] 1) Add the general formula CH in a four-necked flask with a condenser 3 Esters of CHXCOOR, wherein R represents an alkyl group, and the alkyl group includes a halogen-containing alkyl group and a halogen-free alkyl group and a halogen-containing aromatic ring group and a halogen-free aromatic ring group, such as methyl, ethyl, 2, 2,2-trifluoroethyl (CF 3 CH 2 ), phenyl, p-chlorophenyl, pentafluorophenyl, etc., preferably, the general formula is CH 3 X in the ester of CHXCOOR represents halogen, and halogen is Cl;

[0023] 2) then in four-necked flask, add auxiliary agent, catalyst and solvent, auxiliary agent is that general formula is R 1 C(OR 2 ) 3 compound, R 1 for H or CH 3 One of the R 2 for CH 3 or C 2 h 5 One of them, the general formula is R 1 C(OR 2 ) 3 Compounds with the general formula CH 3 The mass ratio of CHXCOOR esters is 0.02-0.2:1. The...

Embodiment 1

[0027] Add 720g of sulfolane, 245g (2.0mol) of methyl 2-chloropropionate, 25g of dodecyltrimethylammonium chloride, 25g of trimethyl orthoacetate, and potassium fluoride into a 2L four-necked flask with a condenser tube. 220.1g, stirred, heated to 120°C, and reacted for 6h. After the reaction, the reaction solution was rectified to obtain 150 g of methyl 2-fluoropropionate with a purity of 99.2% and a yield of 70.2%.

Embodiment 2

[0029] Add DMF1100g, ethyl 2-chloropropionate 273g (2.0mol), tetrabutylammonium bromide 54g, triethyl orthoformate 5.5g, potassium fluoride 255.2g in a 2L four-necked flask with a condenser, and stir , heated to 100°C, and reacted for 12h. After the reaction, rectification gave 176.3 g of ethyl 2-fluoropropionate with a purity of 99.5% and a yield of 66.5%.

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Abstract

The invention discloses a 2-fluoropropionate synthetizing method. The method comprise the steps of 1, adding ester to a four-mouth flask provided with a condenser pipe, wherein the general formula of the ester is CH3CHXCOOR, and R represents alkyl; 2, adding an addition agent, a catalyst and solvent to the four-mouth flask, and then adding a fluorinated reagent and conducting stirring to obtain reaction liquid; 3, heating the reaction liquid to a set temperature, wherein reaction time is 3-16 h; 4, conducting rectification after reaction ends to obtain a 2-fluoropropionate target product. According to the method, cheap 2-CH3CHClCOOR is used as the raw material, and fluorination is conducted with potassium fluoride in the presence of the addition agent to obtain the 2-fluoropropionate. The method has the advantages that the reaction condition is mild, the yield is high, and cost is low. Due to the fact that the addition agent is added, generation of high-boiling by-products can be restrained, and then reaction selectivity is improved.

Description

technical field [0001] The invention relates to a method for preparing fluoroalkyl esters, in particular to a method for synthesizing 2-fluoropropionate. Background technique [0002] Poly 2-fluoroacrylate has the advantages of high glass transition temperature, low surface energy, aging resistance, and low signal attenuation, and can be used in plastic optical fibers, and 2-fluoropropionate is a key intermediate for the synthesis of 2-fluoroacrylate. There are three main routes for the synthesis of 2-fluoropropionate. (1) Take 2-chloropropionate as raw material. According to RecuildestrvauxdesPays-BasdesPays-Bas; (1947); p.424 reported that under the condition of 180~190°C, 2-chloropropionate was exchanged with potassium fluoride to obtain 2-fluoropropionate with a yield of 56%. . CN103044245A reports that 2-chloropropionate and liquid hydrogen fluoride undergo fluorine-chlorine exchange reaction under the catalysis of a catalyst to obtain 2-fluoropropionate with a maxim...

Claims

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Application Information

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IPC IPC(8): C07C67/307C07C69/63
CPCC07C67/307C07C69/63
Inventor 叶立峰王树华余燕汪宇轩
Owner JUHUA GRP
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