Preparation method of 3,3,3-trifluoromethyl propionate

A technology of methyl trifluoropropionate and trifluoropropionaldehyde dimethoxyethane, which is applied in the preparation field of the chemical technology field, can solve the problems of complicated post-processing, few reaction steps, low yield and the like, and achieves post-processing Simple, few reaction steps

Active Publication Date: 2013-06-26
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the technical problems of many reaction steps, low yield and complex post-treatment in the background technology, the purpose of the present invention is to provide a 3,3,3-trifluoropropionic acid with fewer reaction steps and higher reaction yield The preparation method of methyl ester

Method used

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  • Preparation method of 3,3,3-trifluoromethyl propionate
  • Preparation method of 3,3,3-trifluoromethyl propionate

Examples

Experimental program
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Effect test

Embodiment 1

[0016] At room temperature, 25 g of 3,3,3-trifluoropropionaldehyde dimethoxyethane, 2.0 g of hydrochloric acid (36% by mass fraction) and 1 g of V 2 o 5 Add it into the reaction bottle, heat up to 70°C, add 10g of hydrogen peroxide (mass fraction 30%) dropwise under stirring, then react at 70°C for 5 hours, cool, stand still, separate liquid, and collect at 70°C~73°C by atmospheric distillation Distillation obtained 16.8g of a colorless liquid with a purity of 98%, yield 75.0%.

Embodiment 2

[0018] Add 3,3,3-trifluoropropionaldehyde dimethoxyethane at room temperature: 25g, hydrochloric acid (mass fraction 36%): 2.5g, V 2 o 5 : 1.5g in a reaction flask, heated up to 70°C, added dropwise 13g of hydrogen peroxide (mass fraction 30%) under stirring, then reacted at 70°C for 5h, cooled, stood still, separated, and collected by atmospheric distillation at 70°C 17.1 g of a colorless liquid with a purity of 98% was obtained in a fraction at ~73°C, and the yield was 76.0%.

Embodiment 3

[0020] Add 25 g of 3,3,3-trifluoropropionaldehyde dimethoxyethane, 2.5 g of sulfuric acid and 1.2 g of CuCl at room temperature 2 In the reaction bottle, heat up to 70°C, add 12.5g of hydrogen peroxide (mass fraction 30%) dropwise under stirring, then react at 70°C for 5 hours, cool, stand still, separate liquid, and collect at 70°C~ At 73°C, 16.4 g of a colorless liquid with a purity of 98% was obtained, with a yield of 72.3%.

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Abstract

The invention discloses a preparation method of 3,3,3-trifluoromethyl propionate. The method is characterized by adding 3,3,3-trifluoropropionaldehyde dimethoxyethane, a protonic acid and a pro-oxidant to a three-neck flask, raising the temperature to 60-80 DEG C and dropwise adding hydrogen peroxide under stirring to react for 4-8 hours, wherein the mass ratio of 3,3,3-trifluoropropionaldehyde dimethoxyethane to the protonic acid to the pro-oxidant to hydrogen peroxide is 1:(0.04-0.2):(0.04-0.1):(0.1-0.6); the protonic acid is hydrochloric acid or sulfuric acid; and the pro-oxidant is copper chloride, ferric chloride or vanadium pentoxide. The preparation method has the beneficial effects that the preparation method is few in reaction steps and simple in postprocessing; and 3,3,3-trifluoromethyl propionate is prepared only through one-step reaction.

Description

technical field [0001] The invention belongs to a preparation method in the technical field of chemistry, and in particular relates to a preparation method of methyl 3,3,3-trifluoropropionate. Background technique [0002] Methyl 3,3,3-trifluoropropionate can be used as an intermediate in the synthesis of medicines and pesticides, and can also be used as a raw material or intermediate in the synthesis of high-performance fluorine-containing materials. "Convenient synthesis of 3,3,3-trifluoropropanoic acid by hydrolytic oxidation of 3,3,3-trifluoropropanal dimethyl acetate"Journal of fluorine chemistry, 129 (1) 35-39, 2008 discloses a 3,3,3-trifluoro The preparation method of methyl propionate, the method takes 3,3,3-trifluoropropenyl ether as raw material, and prepares the method for 3,3,3-trifluoropropionate methyl ester through three-step reaction, and its reaction steps are as follows: [0003] [0004] First, 3,3,3-trifluoropropenyl ether and methanol are catalyzed b...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/39
Inventor 亢建平吕剑杜咏梅李凤仙王伟马辉吕婧唐晓博张振华惠丰
Owner XIAN MODERN CHEM RES INST
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