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Method for synthesizing 3,3,3-trifluoro-propyl alcohol

A technology of trifluoropropanol and a synthesis method, applied in 3 fields, can solve the problems of difficult separation and purification, low reaction yield and the like, and achieve the effects of high reaction yield and simple post-processing

Inactive Publication Date: 2012-11-07
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the reaction yield of this method is low; and the second step reaction is a water system, trifluoropropanol and water exist azeotrope, and it is difficult to separate and purify the product post-treatment process

Method used

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  • Method for synthesizing 3,3,3-trifluoro-propyl alcohol
  • Method for synthesizing 3,3,3-trifluoro-propyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Under stirring, add 96g of methanol and 80g of sodium hydroxide into the reactor, then add 87.5g of 2-bromo-3,3,3-trifluoropropene, heat up to 70°C, react for 6h, cool to room temperature, and material, the reaction solution was washed three times with 100 g of water to neutrality, and methanol, sodium bromide and sodium hydroxide were removed to obtain 44.1 g of 3,3,3-trifluoropropenyl methyl ether with a yield of 70% and a purity of 98%.

[0020] (2) Add 44.1g of 3,3,3-trifluoropropenyl methyl ether, 66.2g of tributyl phosphate and 4.4g of activated Raney Ni catalyst into the autoclave, the pressure of hydrogen filling is 5MPa, under stirring, heat Raise the temperature to 100°C, react for 6 hours, cool to room temperature, remove the reaction solution, filter the reaction solution, separate the catalyst from the reaction solution, distill the obtained filtrate under normal pressure, collect the fraction at 87-89°C to obtain 3,3,3-trifluoropropane Alcohol 35.0g, y...

Embodiment 2

[0034] (1) Under stirring, add 128g of methanol and 80g of sodium hydroxide into the reactor, then add 87.5g of 2-bromo-3,3,3-trifluoropropene, heat up to 70°C, react for 6h, cool to room temperature, and discharge, The reaction liquid was washed three times with 100 g of water to neutrality, and methanol, sodium bromide and sodium hydroxide were removed to obtain 42.8 g of 3,3,3-trifluoropropenyl methyl ether with a yield of 68.0% and a purity of 98%.

[0035] (2) 42.8g 3,3,3-trifluoropropenyl methyl ether, 51.4g dipropyl carbonate and 2.6g activated Raney Ni catalyst are added in the autoclave, the hydrogen pressure is 5MPa, under stirring, the temperature is raised to 100°C, reacted for 6h, cooled to room temperature, removed the reaction liquid, filtered the reaction liquid, separated the catalyst from the reaction liquid, distilled the obtained filtrate under normal pressure, collected 87-89°C fractions, and obtained 3,3,3-trifluoropropanol 32.2 g, yield 81.5%, purity 98%...

Embodiment 3

[0037] (1) Under stirring, add 128g of methanol and 120g of sodium hydroxide into the reactor, then add 87.5g of 2-bromo-3,3,3-trifluoropropene, heat up to 70°C, react for 6h, cool to room temperature, and discharge, The reaction solution was washed three times with 100 g of water to neutrality, and methanol, sodium bromide and sodium hydroxide were removed to obtain 43.5 g of 3,3,3-trifluoropropenyl methyl ether with a yield of 69.1% and a purity of 98%.

[0038] (2) 43.5g 3,3,3-trifluoropropenyl methyl ether, 55.7g diethyl carbonate and 2.2g activated Raney Ni catalyst are added in the autoclave, the pressure of hydrogen filling is 5MPa, under stirring, the temperature is raised to 70°C, reacted for 6h, cooled to room temperature, removed the reaction liquid, filtered the reaction liquid, separated the catalyst from the reaction liquid, distilled the obtained filtrate under atmospheric pressure, collected 87-89°C fractions, and obtained 3,3,3-trifluoropropanol 30.5 g, yield ...

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Abstract

The invention discloses a method for synthesizing 3,3,3-trifluoro-propyl alcohol. 2-dibromo3,3,3-trifluoropropene serves as the raw material, and the method includes the following steps: adding methanol and alkali in stirring mode, then adding 2-dibromo3,3,3-trifluoropropene, warming to 70 DEG C, reacting for 6h, and obtaining 3,3,3-trifluoropropene-methyl ether by washing reaction liquor, wherein mole ratio of 2-dibromo3,3,3-trifluoropropene: methanol: alkali is 1:(3-8):(2.4-6.2); and (2) adding 3,3,3-trifluoropropene-methyl ether, inorganic ester and activated Raney Ni catalysts into an autoclave, leading hydrogen pressure to be 5MPa, stirring to lead temperature to rise to 60-120 DEG C, reacting for 4-8h, and filtering and distilling reaction liquor to obtain 3,3,3-trifluoro-propyl alcohol, wherein mass ratio of 3,3,3-trifluoropropene-methyl ether: inorganic ester: catalysts is 1:(1.2-2.0):(0.05-0.2). The method is mainly used for preparing 3,3,3-trifluoro-propyl alcohol.

Description

technical field [0001] The present invention relates to a kind of synthetic method of 3,3,3-trifluoropropanol, especially a kind of synthesis method of 3,3,3-trifluoropropanol with 2-bromo 3,3,3-trifluoropropene as raw material Preparation. Background technique [0002] 3,3,3-Trifluoropropanol 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 materials. "Investigation of the factors controlling the regioselectivity of the hydroboration of fluoroolefins" Chemical communication, 2002, 386-387 discloses a preparation method of 3,3,3-trifluoropropanol, which uses trifluoropropene as raw material through two Step reaction preparation obtains 3,3,3-trifluoropropanol, and reaction steps are as follows: [0003] [0004] Firstly, trifluoropropene was reacted with dibromoborane to prepare boron compound, and then hydrolyzed and oxidized to obtain trifluoropropan...

Claims

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Application Information

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IPC IPC(8): C07C31/38C07C29/17C07C29/132
Inventor 杜咏梅吕剑毛伟谷玉杰孙道安王博秦越李春迎赵锋伟王为强
Owner XIAN MODERN CHEM RES INST
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