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Production process of 3,3,3-trifluoro- propyl aldehyde

A technology for trifluoropropionaldehyde and trifluoropropene, which is applied in the field of preparing 3,3,3-trifluoropropionaldehyde, and can solve the problems that trifluoromethyl iodide raw materials are not readily available, expensive, and the like

Inactive Publication Date: 2015-06-03
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, trifluoromethyl iodide raw material is not easy to get, expensive

Method used

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  • Production process of 3,3,3-trifluoro- propyl aldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Lower the temperature of the reaction bottle to -15°C to -10°C, add 104g of 35% mass concentration of hydrochloric acid, 5.6g of iron powder, and 453g of 30% mass concentration of hydrogen peroxide under stirring, and continue stirring for 1 hour to prepare an oxidizing reagent. Add 158g of 1,1,1-trifluoro-3,3-dimethoxypropane into another reaction flask, then heat it to 100°C under stirring, slowly add the oxidizing reagent dropwise, after the dropwise addition, continue to react for 2 more Hours, the reaction is over, cooled, and then distill off the fraction at 40-70°C, and then collect the fraction at 56°C by rectification to obtain 78g of 3,3,3-trifluoropropanal, 3,3,3-trifluoropropanal The yield of propionaldehyde is 69.6%.

[0033] According to the nuclear magnetic structure identification, the prepared product is indeed 3,3,3-trifluoropropanal, the data are as follows:

[0034] MS: m / z112 (M + ), 64(100).

[0035] 1 HNMR (CDCl 3 ): δ / ppm3.22 (m, 2H), 9.72 (...

Embodiment 2

[0037] Lower the temperature of the reaction flask to -15°C to -10°C, add 104g of hydrochloric acid with a mass concentration of 35% under stirring, V 2 o 5 9g, 453g of hydrogen peroxide at 30% mass concentration, and continued to stir for 1 hour to prepare the oxidizing reagent. Add 158g of 1,1,1-trifluoro-3,3-dimethoxypropane into another reaction flask, then heat it to 100°C under stirring, slowly add the oxidizing reagent dropwise, after the dropwise addition, continue to react for 2 more Hours, the reaction was over, cooled, and then distilled out the fraction at 40-70°C, and then collected the fraction at 56°C by rectification to obtain 89g of 3,3,3-trifluoropropanal, 3,3,3-trifluoropropanal The yield of propionaldehyde is 79.4%.

Embodiment 3

[0039]Lower the temperature of the reaction flask to -15°C to -10°C, add 104g of 35% mass concentration hydrochloric acid, FeCl 3 8g, 453g of hydrogen peroxide at 30% mass concentration, and continued to stir for 1 hour to prepare the oxidizing reagent. Add 158g of 1,1,1-trifluoro-3,3-dimethoxypropane into another reaction flask, then heat it to 100°C under stirring, slowly add the oxidizing reagent dropwise, after the dropwise addition, continue to react for 2 more Hours, the reaction is over, cooled, and then distill off the fraction at 40-70°C, and then collect the fraction at 56°C by rectification to obtain 96g of 3,3,3-trifluoropropanal, 3,3,3-trifluoropropanal The yield of propionaldehyde is 85.7%.

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Abstract

The invention discloses a method for preparing 3,3,3-trifluoro- propyl aldehyde. 1,1,1-trifluoro-3,3-dimethoxy propane is taken as a raw material to generate the 3,3,3-trifluoro-propyl aldehyde by the effect of an oxidizing reagent. The method disclosed by the invention is novel in synthetic route, high in reaction yield and environment-friendly, and the prepared 3,3,3-trifluoro-propyl aldehyde can be used as a midbody for medicines and pesticides.

Description

technical field [0001] The invention relates to a production process for preparing 3,3,3-trifluoropropanal. Background technique [0002] 3,3,3-Trifluoropropionaldehyde is a very useful organic chemical and biochemical reagent, which can be used as an intermediate in medicine and pesticides and in the production of high-performance materials, such as raw materials or synthetic intermediates for fluoropolymers, It occupies an important position in fluorine-containing aliphatic compounds. [0003] Regarding the method for preparing 3,3,3-trifluoropropionaldehyde, following reports are arranged in the prior art: [0004] (1) Trifluoropropenyl ether as raw material [0005] U.S. Patent No. 6,111,139 discloses a method for preparing 3,3,3-trifluoropropanal, which uses 1-chloro-3,3,3-trifluoropropene and metal alkoxide in alcohol (ROH, R is C1 -C4 alkyl) in the reaction, the intermediate product fluoroether CF is obtained first 3 CH=CH-OR and CF 3 CH 2 CH(OR) 2 , and then r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/14C07C45/30C07C45/27
CPCC07C45/30C07C45/27C07C47/14
Inventor 肖恒侨韩国庆徐卫国盛楠陈明炎项文勤
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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