A kind of preparation method of 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 that sodium methoxide is easy to oxidize and hydrolyze and deteriorate, cannot be scaled up for industrial production, and it is difficult to control the reaction temperature, etc. problems, to achieve the effect of easy control of reaction temperature, avoiding high temperature and pressurized conditions, and solving stirring problems
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Embodiment 1
[0093] Example 1: Preparation process of pentafluorophenol
[0094] Step 1: Preparation of pentafluoroanisole (etherification)
[0095] Hexafluorobenzene (146g) was added to a 1L four-neck flask, and methanol solution of potassium hydroxide (46g potassium hydroxide, 138g methanol) was added dropwise at 35-45°C, and the reaction was continued for 5-10 hours after the addition. After the reaction, the temperature was lowered to room temperature, water was added, the layers were separated, and the organic layer was rectified to collect fractions at 138-139° C. to obtain pentafluoroanisole (127 g) as a colorless and transparent liquid. The yield was 82%.
[0096] Step 2: Preparation of pentafluorophenol (pyrolysis)
[0097] Add 1,2-dichloroethane (190g) and aluminum trichloride (95g) to a 1L four-neck flask, add pentafluoroanisole (117g) dropwise at 50-60°C, and continue the reaction for 4 hours after the addition. After the reaction, it was cooled to room temperature, water was added, ...
Embodiment 2
[0100] Example 2: Preparation process of pentafluorophenol (preparation of pentafluorophenol by one-step method of hexafluorobenzene)
[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, the temperature was reduced to room temperature, water was added, and the solvent was evaporated. The aqueous layer was acidified with hydrochloric acid and extracted with methyl tert-butyl ether. The organic layers were combined and then rectified. The solvent was first evaporated, and then the 142-144°C fraction was collected. The pentafluorophenol (69g) 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 process is as follows:
[0103]
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