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Preparation method for 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butyl-1-ol

A technology of trifluoromethyl and tetrahydrofuran, which is applied in the field of preparing 3,4,4,4-tetrafluoro-3-butan-1-ol, can solve the problems of high yield, poor surface activity, and insufficient production capacity, and achieve The principle and synthesis process are simple, the requirements for production equipment are low, and the effect of reaction conditions is low

Inactive Publication Date: 2015-08-26
苏州久王环保科技股份有限公司 +1
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0003] At present, the production of fluorocarbon alcohols mainly includes three processes: electrolytic fluorination, oligomerization, and telomerization. The first two methods have many by-products, low yield, difficult to solve pollution, and poor surface activity; telomerization The reaction method has few by-products and high yield, and has been monopolized by a few multinational companies such as DuPont and Daikin. At present, the low-temperature and low-pressure telomerization method that does not extract pentafluoroiodoethane is used in China to produce fluorocarbon alcohols, but the production capacity is seriously insufficient. Demand is still mainly dependent on imports. Therefore, we have developed a method for preparing 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butan-1-ol, which requires low reaction conditions and is easy to operate. and increased productivity

Method used

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Examples

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preparation example Construction

[0014] attached figure 1 The method for preparing 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butan-1-ol according to the present invention:

[0015] First prepare the Grignard reagent, get 20ml of anhydrous tetrahydrofuran solvent and pour it into a three-neck flask, use nitrogen as a protective gas, add 0.022mol (0.528g) of magnesium powder, add a small amount of iodine as an initiator, and carry out magnetic stirring. 0.02 mol (4.98 g) of 2-bromoheptafluoropropane was added dropwise under heating conditions, and magnetically stirred for a period of time to obtain the Grignard reagent for use.

example 1

[0016] Example 1 (reaction temperature T=10 DEG C):

[0017] Take a four-neck bottle, take 50ml of tetrahydrofuran solvent, add 0.02mol (0.88g) of ethylene oxide, install a thermometer and a condensation reflux device, and control the temperature at 10°C, slowly add 0.03mol of Grignard reagent dropwise And carry out magnetic stirring reaction. After the dropwise addition, reflux reaction at 10°C for 0.5h. After the reaction, first heat up to evaporate the solvent, and then distill under reduced pressure at 80°C to distill the product 3,4,4,4-tetrafluoro- The mass of 3-(trifluoromethyl)butan-1-ol was distilled off to obtain 3.62 g, and the yield (calculated based on theoretical yield) was 84.50%.

[0018] Example 2-16, the reaction temperature is 10°C, 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butan-1-ol, the raw materials and reagents used are as follows:

[0019] example

[0020] Reaction temperature / ℃

[0021] example

example 17

[0022] Example 17 (reaction temperature T=5°C):

[0023] Take a four-neck bottle, take 50ml of tetrahydrofuran as a solvent, add 0.02mol (0.88g) of ethylene oxide, install a thermometer and a condensation reflux device on the rack, control the system temperature at 5°C, and slowly add 0.03mol dropwise to prepare Grignard reagent and magnetic stirring reaction, after the dropwise addition, reflux reaction at 5°C for 0.5h. Tetrafluoro-3-(trifluoromethyl)butan-1-ol was distilled off to obtain a mass of 3.74 g, and the yield (calculated based on theoretical yield) was 87.37%.

[0024] Examples 18-32, the reaction temperature is 5°C, 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butan-1-ol, the raw materials and reagents used are as follows:

[0025]

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Abstract

The invention relates to a preparation method for 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butyl-1-ol. The method comprises the following steps: pouring an anhydrous tetrahydrofuran solvent into a three-necked bottle, adding magnesium powder with nitrogen as protective gas, and adding iodine as an initiator at the same time, then carrying out magnetic stirring, dropwise adding 2-bromoheptafluoropropane under heating, and carrying out magnetic stirring reaction so as to prepare a Grignard reagent; and adding a tetrahydrofuran solvent and ethylene oxide as raw materials into a four-necked bottle, dropwise adding the prepared Grignard reagent and carrying out magnetic stirring reaction, then carrying out reflux reaction, distilling the obtained product so as to obtain a final product--the 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butyl-1-ol. The preparation method for the 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butyl-1-ol provided by the invention has the advantages of simple principle and synthetic process, low requirements on reaction conditions, convenient and safe operation, low requirement on production equipment, applicability to large-scale production and high yield of 95.5%.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to a method for preparing 3,4,4,4-tetrafluoro-3-(trifluoromethyl)butan-1-ol. Background technique [0002] As an important intermediate of organic fluorine chemical industry, fluorocarbon alcohol has unique chemical stability, corrosion resistance, flame retardancy, hydrophobicity, oil repellency, antifouling and many other characteristics; its application has penetrated into textiles, military industry, electronics, Aerospace, anti-corrosion, chemical industry, surface protection and other social production and living fields, widely used in industrial and commercial activities such as high-end clothing, advanced construction, aircraft manufacturing, precision machining, cultural relics protection, high-voltage insulation, ocean development, coating coatings, etc. It plays an immeasurable role in human production and life; [0003] At present, the production of fluorocarbon alcoh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/36C07C31/38
CPCC07C29/36C07C31/38
Inventor 张超智王宏明顾智杰
Owner 苏州久王环保科技股份有限公司
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