Unlock instant, AI-driven research and patent intelligence for your innovation.

Synthesis method of 2,3,3,3-tetrafluoropropionate

A technology of tetrafluoropropionate and synthesis method, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of no cost advantage, high price, and labor protection requirements for polluting the environment Low price, wide application range, simple and easy reaction operation and post-processing

Inactive Publication Date: 2017-01-04
赵满良
View PDF10 Cites 10 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Japanese patent JP57085339 describes the use of 1,1,2,3,3,3-hexafluoropropene (Ⅳ) as the starting material, first reacting with methanol to generate compound V, and then preparing 2,3,3,3 through defluorination reaction - The method of methyl tetrafluoropropionate (II), which has mild reaction conditions and is easy to operate, but the starting material 1,1,2,3,3,3-hexafluoropropene (IV) is expensive and is a gas , there is no cost advantage in industrial production and pressure vessels are required, which is not conducive to large-scale preparation
The hydrofluoric acid produced by the reaction is also an extremely toxic compound, polluting the environment and requiring high labor protection

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthesis method of 2,3,3,3-tetrafluoropropionate
  • Synthesis method of 2,3,3,3-tetrafluoropropionate
  • Synthesis method of 2,3,3,3-tetrafluoropropionate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Preparation of methyl 2,3,3,3-tetrafluoropropionate

[0030] Put water (300ml), methanol (500ml), N,N-diethyl-2,3,3,3-tetrafluoropropionamide (900g, 4.47mol), 37% hydrochloric acid (1000ml) into the reaction flask , The temperature was raised to 130°C and refluxed for 10 hours. After the reaction was completed, atmospheric distillation was carried out. The fractions around 100°C were collected to obtain methyl 2,3,3,3-tetrafluoropropionate with a yield of 93% and a purity of 98%.

Embodiment 2

[0031] Example 2: Preparation of ethyl 2,3,3,3-tetrafluoropropionate

[0032] Put water (300ml), ethanol (500ml), N,N-diethyl-2,3,3,3-tetrafluoropropionamide (900g, 4.47mol), 37% hydrochloric acid (1000ml) into the reaction flask , The temperature was raised to 130°C and refluxed for 10 hours. After the reaction was completed, atmospheric distillation was carried out. The fractions around 110°C were collected to obtain ethyl 2,3,3,3-tetrafluoropropionate with a yield of 95% and a purity of 98.2%.

Embodiment 3

[0033] Example 3: Preparation of ethyl 2,3,3,3-tetrafluoropropionate

[0034] Mix water (300ml), ethanol (500ml), N,N-diethyl-2,3,3,3-tetrafluoropropionamide (900g, 4.47mol), 37% hydrochloric acid (1000ml), sodium metaaluminate ( 10g) Put it in a reaction flask, heat up to 130°C and reflux for 10 hours. After the reaction is complete, distill under normal pressure. Collect fractions around 110°C to obtain ethyl 2,3,3,3-tetrafluoropropionate with a yield of 96% and purity 98.5%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the technical field of organic chemistry and provides a synthesis method of 2,3,3,3-tetrafluoropropionate. According to the synthesis method, a N,N-disubstituted-2,3,3,3-tetrafluoropropionamide pure product or a mixture containing 0.1 percent to 99.99 percent of the N,N-disubstituted-2,3,3,3-tetrafluoropropionamide is used as a starting raw material, and is hydrolyzed and treated by an esterification one-pot method in the presence of acid or alkali and corresponding alcohol to obtain the 2,3,3,3-tetrafluoropropionate. The 2,3,3,3-tetrafluoropropionate (II) is synthesized through adopting the simple and easy-to-operate one-pot method; an applicable range is wide and conditions are moderate; the synthesis method is suitable for industrial production.

Description

Technical field [0001] The invention belongs to the technical field of organic chemistry, and is a synthesis method of 2,3,3,3-tetrafluoropropionate. Background technique [0002] 2,3,3,3-Tetrafluoropropionate is an important fluorine-containing intermediate, which is widely used in the fields of pesticides, medicine, and materials science. [0003] [0004] Japanese patent JP57085339 describes that 1,1,2,3,3,3-hexafluoropropene (IV) is used as a starting material, firstly reacted with methanol to produce compound V, and then defluorinated to produce 2,3,3,3 -The method of methyl tetrafluoropropionate (II), which has mild reaction conditions and easy operation, but the starting material 1,1,2,3,3,3-hexafluoropropene (IV) is expensive and gas , There is no cost advantage in industrial production and pressure vessels are needed, which is not conducive to large-scale production. The hydrofluoric acid produced by the reaction is also a highly toxic compound, which pollutes the enviro...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/20C07C69/63
CPCC07C67/20C07C69/63
Inventor 赵满良
Owner 赵满良