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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  • 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, trifluoropropa

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
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Example Embodiment

[0018] Example 1

[0019] (1) Under stirring, add 96g methanol and 80g sodium hydroxide into the reactor, then add 87.5g 2-bromo 3,3,3-trifluoropropene, heat to 70℃, react for 6h, cool to room temperature, 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, fill the autoclave with a hydrogen pressure of 5MPa, stir and heat Warm up 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 filtrate at atmospheric pressure, collect the 87-89°C fraction to obtain 3,3,3-trifluoropropane The alcohol is 35.0g, the yield is 86.0%, the pu...

Example Embodiment

[0033] Example 2

[0034] (1) Under stirring, add 128g methanol and 80g sodium hydroxide into the reactor, then add 87.5g 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 until it was neutral to remove methanol, sodium bromide and sodium hydroxide 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) Add 42.8g of 3,3,3-trifluoropropenyl methyl ether, 51.4g of dipropyl carbonate and 2.6g of activated Raney Ni catalyst into the autoclave, fill the autoclave with a hydrogen pressure of 5MPa, stir and heat to React at 100°C for 6 hours, cool to room temperature, remove the reaction solution, filter the reaction solution, separate the catalyst from the reaction solution, and distill the filtrate at atmospheric pressure to collect the 87-89°C fraction to obtain 3,3,3-trifluoropropanol 32.2 g, the yield is 81.5...

Example Embodiment

[0036] Example 3

[0037] (1) Under stirring, add 128g methanol and 120g sodium hydroxide into the reactor, then add 87.5g 2-bromo 3,3,3-trifluoropropene, raise the temperature to 70°C, react for 6h, cool to room temperature, discharge, The reaction solution was washed three times with 100 g of water until it was neutral to remove methanol, sodium bromide and sodium hydroxide 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) Add 43.5g of 3,3,3-trifluoropropenyl methyl ether, 55.7g of diethyl carbonate and 2.2g of activated Raney Ni catalyst into the autoclave, fill the autoclave with a hydrogen pressure of 5MPa, stir and heat to React at 70°C for 6 hours, cool to room temperature, remove the reaction solution, filter the reaction solution, separate the catalyst from the reaction solution, and distill the filtrate at atmospheric pressure to collect the 87-89°C fraction to obtain 3,3,3-trifluoropropanol 30.5 g, the 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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