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A kind of synthetic method of hexafluoro-1-butanol

A synthetic method and technology of butanol, applied in the direction of organic chemistry, oxygen-containing functional group reduction preparation, etc., can solve the problem of not being able to obtain a single product, and achieve the effects of mature reaction technology, conventional raw materials, and mild reaction conditions

Active Publication Date: 2020-12-08
湖南有色郴州氟化学有限公司
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] There is a common defect in the above three telomerization reaction methods, the prepared hexafluorobutanol is a mixture of hexafluoro-1-butanol and hexafluoro-2-butanol, and a single product cannot be obtained

Method used

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  • A kind of synthetic method of hexafluoro-1-butanol
  • A kind of synthetic method of hexafluoro-1-butanol
  • A kind of synthetic method of hexafluoro-1-butanol

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preparation example Construction

[0030] The invention provides a synthetic method of hexafluoro-1-butanol, comprising:

[0031] The compound of the formula (I) and hydrogen undergo an addition reaction under the catalysis of a noble metal catalyst to obtain hexafluoro-1-butanol;

[0032]

[0033] The compound of the formula (I) structure provided by the present invention is preferably prepared according to the method of the present invention:

[0034] Hexafluoropropylene reacts with formaldehyde to obtain a compound of formula (I).

[0035] More preferably, hexafluoropropylene and formaldehyde undergo addition reaction in a solvent to prepare the compound of formula (I).

[0036] The present invention does not limit the sources of the hexafluoropropylene and formaldehyde, which can be commercially available.

[0037] According to the present invention, the molar ratio of the hexafluoropropylene to formaldehyde is preferably (1-6):1; more preferably (1-3):1; and most preferably 3:1.

[0038] The reaction...

Embodiment 1

[0062] Add 60.0g of hexafluoropropylene and 50g of hydrogen fluoride into a 500ml reaction kettle, mix well under mechanical stirring, then raise the temperature of the reaction bottle to 50°C, slowly inject 12g of formaldehyde into the reaction kettle with a metering pump, after the feeding of formaldehyde is completed, continue React for 12 hours, then stop the reaction, remove hydrogen fluoride by distillation, neutralize the crude product with 10% sodium hydroxide solution to a pH value of 7-8, separate phases, dry the organic phase with anhydrous sodium sulfate, and then carry out rectification to the crude product After purification, 64.8 g of 1-trifluoromethyl-trifluorooxetane was obtained with a yield of 90%.

[0063] The obtained 1-trifluoromethyl-trifluorooxetane 64.8g is subjected to hydrogenation hydrogenation. First, the reactor is evacuated and replaced with nitrogen for three times, and the air in the reactor is completely replaced, and then 1g of palladium carbo...

Embodiment 2

[0066] Add 60.0g of hexafluoropropylene and 50g of hydrogen fluoride into a 500ml reaction kettle, mix well under mechanical stirring, then raise the temperature of the reaction bottle to 50°C, slowly inject 12g of formaldehyde into the reaction kettle with a metering pump, after the feeding of formaldehyde is completed, continue React for 12 hours, then stop the reaction, remove hydrogen fluoride by distillation, neutralize the crude product with 10% sodium hydroxide solution to a pH value of 7-8, separate phases, dry the organic phase with anhydrous sodium sulfate, and then carry out rectification to the crude product After purification, 64.8 g of 1-trifluoromethyl-trifluorooxetane was obtained with a yield of 90%.

[0067] The obtained 1-trifluoromethyl-trifluorooxetane 64.8g is subjected to hydrogenation hydrogenation. First, the reactor is evacuated and replaced with nitrogen for three times, and the air in the reactor is completely replaced, and then 1g of platinum carbon...

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Abstract

The invention provides a synthetic method of hexafluoro-1-butanol. The synthetic method of hexafluoro-1-butanol comprises the following step: carrying out an addition reaction on a compound of a structure as shown in a formula (I) and hydrogen under catalyst of a noble metal catalyst to obtain hexafluoro-1-butanol. By taking the compound of the structure as shown in the formula (I): 1-trifluoromethyl-trifluorooxetane as an initial raw material, hexafluoro-1-butanol is obtained by means of hydrogenation under the special catalyst. The method is mature in reaction technology of steps, conventional in raw material and mild in reaction condition, and is an advantageous technical line. Experimental results verify that the total yield of hexafluoro-1-butanol is greater than 87% and the purity isgreater than 99%.

Description

technical field [0001] The invention relates to the technical field of fine fluorine chemicals, in particular to a synthesis method of hexafluoro-1-butanol. Background technique [0002] Hexafluorobutanol is an important aliphatic fluorine-containing intermediate, which has good solubility and surface activity, and is mainly used as a solvent, surfactant, and intermediate for the synthesis of dyes and pesticides. [0003] As a solvent, hexafluorobutanol is suitable for the manufacture of information recording media (discs such as CD-R, DVD-R, etc.) including substrates and recording layers suitable for writing and / or reading built on them, and can also be used for films The manufacture of photosensitive materials. An information recording medium containing a substrate and a recording layer suitable for writing and / or reading constructed thereon can be obtained by dissolving the dye in a hexafluorobutanol solvent and using the solution to perform a series of conventional ope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/132C07C31/38
CPCC07C29/132C07D305/08C07C31/38
Inventor 王刚张振华
Owner 湖南有色郴州氟化学有限公司
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