Preparation method for pentafluorophenol

A technology of pentafluorophenol and pentafluoroanisole, which is applied in the preparation of organic compounds, ether preparation, chemical instruments and methods, etc. It can solve the problem of easy oxidation and hydrolysis of sodium methoxide, inability to scale up industrial production, difficulty in controlling reaction temperature, etc. problems, to achieve the effect of easy control of reaction temperature, avoiding high temperature and pressurized conditions, and solving stirring problems

Active Publication Date: 2015-11-04
KINGCHEM LIAONING CHEMICAL CO LTD
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Problems solved by technology

[0011] 1) Hexafluorobenzene reacts with sodium methoxide to obtain pentafluoroanisole, which is then cracked with hydroiodic acid to obtain pentafluorophenol: the sodium methoxide used is easy to oxidize and hydrolyze and deteriorate, and the hydroiodic acid used is expensive
[0012] 2) Pentafluorophenetole is obtained by reacting hexafluorobenzene with potassium hydroxide and ethanol under high pressure at 120°C. The etherification reaction temperature is high, high-pressure equipment is required, and the product yield is low
[0013] 3) Hexafluorobenzene and sodium methoxide are refluxed in methanol to obtain pentafluoroanisole, and then cracked with aluminum trichl

Method used

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  • Preparation method for pentafluorophenol
  • Preparation method for pentafluorophenol
  • Preparation method for pentafluorophenol

Examples

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Embodiment 1

[0093] Embodiment 1: the preparation technology of pentafluorophenol

[0094] Step 1: Preparation of pentafluoroanisole (etherification)

[0095] Add hexafluorobenzene (146g) into a 1L four-neck flask, add potassium hydroxide methanol solution (potassium hydroxide 46g, methanol 138g) dropwise at 35-45°C, and continue the reaction for 5-10 hours after the addition is complete. After the reaction, cool down to room temperature, add water, separate layers, rectify the organic layer, and collect fractions at 138-139°C to obtain pentafluoroanisole (127g), which is a colorless transparent liquid. Yield 82%.

[0096] Step 2: Preparation (cracking) of pentafluorophenol

[0097] Add 1,2-dichloroethane (190g) and aluminum trichloride (95g) into a 1L four-neck flask, add pentafluoroanisole (117g) dropwise at 50-60°C, and continue the reaction for 4 hours after the addition is completed. After the reaction, cool down to room temperature, add water, separate layers, rectify the organic ...

Embodiment 2

[0100] Embodiment 2: the preparation technology of pentafluorophenol (hexafluorobenzene one-step method prepares pentafluorophenol)

[0101] Add tert-butanol (500g), potassium hydroxide (75g) and hexafluorobenzene (100g) into a 2L four-neck flask, and react at 60-70°C for 3 hours. After the reaction, cool down to room temperature, add water, distill off the solvent, acidify the aqueous layer with hydrochloric acid, extract with methyl tert-butyl ether, combine the organic layers and rectify, distill off the solvent first, and then collect fractions at 142-144°C. Pentafluorophenol (69 g) was obtained as a white to light brown solid with a melting point of 34-36° C. and a yield of 70%.

[0102] The synthetic route of pentafluorophenol in this preparation technology is as follows:

[0103]

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Abstract

The invention relates to a preparation method for pentafluorophenol. By taking hexafluorobenzene as an initial raw material, pentafluorophenol is prepared through etherification reaction and cracking reaction or by taking hexafluorobenzene as the initial raw material, pentafluorophenol is prepared by virtue of a one-step method. The preparation method provided by the invention does not need high temperature and pressurization, is less in energy consumption, and does not use expensive hydroiodic acid, so that the cost of the raw materials is low. Moreover, wastewater generated by etherification reaction is less, so that the preparation method is environmental-friendly; Cracking is carried out in a solvent, the material stirring effect is good, the reaction temperature is easy to control, and industrialization is easy to implement.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of polyfluorophenol, more specifically to a preparation method of pentafluorophenol. Background technique [0002] Pentafluorophenol (Pentafluorophenol, PFP), also known as 2,3,4,5,6-pentafluorophenol, pentafluorophenol, its molecular formula is C 6 HF 5 O, the molecular weight is 184.06, and the CAS registration number is 771-61-9. Pentafluorophenol is a white crystal, easy to absorb water, with a melting point of 34-36°C and a boiling point of 143°C. It is soluble in water, but its solubility is not large, and it is weakly acidic. Its chemical structure is as follows: [0003] [0004] Pentafluorophenol is an important intermediate, which is mainly used in the preparation of pharmaceutical, liquid crystal and polymer material intermediates. For example, in the fields of medicine and pesticides, pentafluorophenol is mostly used to prepare pentafluorophe...

Claims

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Application Information

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IPC IPC(8): C07C39/27C07C37/055C07C37/02
CPCC07C37/02C07C37/055C07C41/01C07C39/27C07C43/225
Inventor 赵阳李振威付立民李德刚李文捷刘广生
Owner KINGCHEM LIAONING CHEMICAL CO LTD
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