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A kind of synthetic method of 1-hydroxypyrene

A synthetic method and technology of hydroxypyrene, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of reduced reaction yield, unsatisfactory effect, troublesome drying and fine-tuning, etc., and achieve simplified operation steps, have commercial application value, and reduce the effect of side reactions

Active Publication Date: 2022-04-26
福建福瑞明德药业有限公司
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  • Description
  • Claims
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Problems solved by technology

In this method, sodium pyrene-1-sulfonate cannot be dissolved in molten sodium hydroxide, so it is necessary to grind the dry powder of sodium pyrene-1-sulfonate before feeding, because sodium pyrene-1-sulfonate belongs to condensed ring aromatic hydrocarbon compound , the toxicity is very high, so the process of drying and grinding is very troublesome, even so, the effect is not ideal, and the yield is very low; in addition, the melting point of sodium hydroxide is 320 ° C, and the reaction temperature is too high, which will increase the side reactions , not only reduces the reaction yield, but also brings pressure to the subsequent refining and purification

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0016] Dissolve 35.7 kg of pyrene in 6 times the weight of tetrachloroethane, cool to 0°C, dissolve 22.4 kg of chlorosulfonic acid in the same amount of tetrachloroethane, and drop into pyrene at 0-5°C Tetrachloroethane solution, and stirred at 10-20 ° C for 1.5-2.0 hours, pour the resulting gray-green paste into 180 kg of ice water, distill off tetrachloroethane under reduced pressure, and filter off a small amount of unreacted Pyrene, 27 kg of sodium sulfate was added to the filtrate to heat up and reflux for 15 hours to generate pyrene-1-sulfonic acid sodium salt that was easy to filter, filter, and wash with an appropriate amount of water to obtain a water-containing wet product of pyrene-1-sodium sulfonate. How much can be controlled by the time of suction filtration, the moisture content of the wet product of sodium pyrene-1-sulfonate obtained by suction filtration is about 40%-70%, and the yield of this step is 90-95%.

Embodiment 2

[0018] Dissolve 35.7 kg of pyrene in 6 times the weight of tetrachloroethane, cool to 0°C, dissolve 22.4 kg of chlorosulfonic acid in the same amount of tetrachloroethane, and drop into pyrene at 0-5°C Tetrachloroethane solution, and stirred at 10-20 ° C for 1.5-2.0 hours, pour the resulting gray-green paste into 180 kg of ice water, distill off tetrachloroethane under reduced pressure, and filter off a small amount of unreacted Pyrene, add 30% sodium hydroxide aqueous solution dropwise to the filtrate, adjust the pH value to 10.0, heat up and reflux for 15 hours, generate pyrene-l-sulfonic acid sodium salt that is easy to filter, centrifuge, and wash with appropriate amount of water to obtain pyrene-1 -The water-containing wet product of sodium sulfonate, the water content can be controlled by the centrifugation time, the water content of the water-containing wet product of pyrene-1-sodium sulfonate obtained by centrifugal method is about 10%-50%, and the pyrene-1-sulfonate ob...

Embodiment 3

[0020] Continue to dry the sodium pyrene-1-sulfonate obtained in Example 2 at 80°C, and grind it into powder for later use. Add 150 kg of sodium hydroxide to the reactor, stir and raise the temperature, and the temperature rises to about 300°C. Add 50Kmol of pyrene-l-sodium sulfonate that has been dried and ground into powder in batches, and react at a temperature of about 300-320°C for 1 hour. Cool down, slowly add 350 kg of water dropwise, and then add dropwise 30% hydrochloric acid to adjust the pH value of the solution to about 3.0. Cool to room temperature and filter with suction, wash the filter cake with a large amount of water, dry to obtain the crude product, first purify by vacuum sublimation, then decolorize with 15 times of ethyl acetate at 60°C for 1 hour, filter, evaporate most of the solvent from the filtrate, reduce Heat at about 10°C, keep warm for 1 hour, filter, and dry at 70°C to obtain 1-hydroxypyrene. This step yield is 25%.

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Abstract

The present invention relates to a kind of synthetic method of 1-hydroxypyrene, this method is fed into the strong alkali of molten state with the aqueous wet product of pyrene-1-sulfonate sodium to react, obtains 1-hydroxypyrene, the advantage of this method is, has It is beneficial to the dispersion of pyrene-1-sodium sulfonate in the reaction system, and simultaneously reduces the reaction temperature, reduces side reactions, improves the yield of the reaction, and simplifies the purification method of the product.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a method for synthesizing a synthetic material intermediate 1-hydroxypyrene. Background technique [0002] 1-Hydroxypyrene is an intermediate of synthetic materials, and can be used as a catalyst for chemical reactions, as a raw material for OLED displays, and other fields. [0003] The literature on the synthesis method of 1-hydroxypyrene has been reported: the document "Preparation of 1-hydroxypyrene and its mass spectrometry analysis" (Environmental Science, Volume 13, No. 4, 1992, P27-30) reported the synthesis of 1-hydroxypyrene First, pyrene is used as raw material to react with chlorosulfonic acid to generate pyrene-1-sodium sulfonate, and then finely ground pyrene-sodium sulfonate dry powder is reacted with molten sodium hydroxide to generate 1-hydroxypyrene, and finally the obtained product is purified by sublimation method product. In this method, sodium pyrene-1-sulfona...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/04C07C39/12
CPCC07C37/04C07C2603/50C07C39/12
Inventor 任建强张建黄建龙何本雄
Owner 福建福瑞明德药业有限公司
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