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Synthetic method of p-iodophenol

A synthetic method, the technology of p-iodophenol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as complex production, and achieve the effects of low cost, simplified process, and high yield

Pending Publication Date: 2022-04-15
营口兴福化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis of p-iodophenol, the drug intermediate of p-iodophenoxyacetic acid, has a long technical process chain and complicated production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] P-iodophenol synthetic method, comprises the following steps:

[0015] Add 40 grams of sodium hydroxide and 250 grams of water into the reaction kettle, then add 25 grams of phenol and 100 grams of methanol into the reaction kettle, and then lower the temperature. The methanol solution for dissolving iodine, the methanol solution for dissolving iodine is a mixture of iodine and methanol with a mass ratio of 1:5, after the dropwise addition, keep stirring for 2 hours, take a sample to detect that the mass fraction of phenol is less than 3%, and then heat up to Distill methanol at 70°C, add 100g of concentrated hydrochloric acid with a mass fraction of 31% for acidification, keep warm for 1 hour at 40°C, then cool down to 15°C for centrifugation to obtain 40g of solid crude product, use 60g for centrifugation Rinse with water twice.

[0016] Add 40 grams of the solid crude product obtained by centrifugation into 200 grams of petroleum ether, recrystallize at 100 ° C, and...

Embodiment 2

[0018] P-iodophenol synthetic method, comprises the following steps:

[0019] Add 35 grams of sodium hydroxide and 225 grams of water into the reaction kettle, then add 15 grams of phenol and 100 grams of methanol into the reaction kettle, and then lower the temperature. 150 grams of methanol solution for dissolving iodine, the methanol solution for dissolving iodine is a mixture of iodine and methyl alcohol with a mass ratio of 1:5, after the dropwise addition, insulated and stirred for 2 hours, and the mass fraction of phenol detected by sampling is less than 3%, Then heat up to 70°C, distill the methanol clean, add 58.5 g of concentrated hydrochloric acid with a mass fraction of 31% for acidification, keep it warm for 1 hour at 40°C, then cool down to 10°C for centrifugation to obtain a solid crude product, which is centrifuged with 50 grams of water twice rinse.

[0020] The solid crude product obtained by centrifugation was added to petroleum ether whose mass was 5 times...

Embodiment 3

[0022] P-iodophenol synthetic method, comprises the following steps:

[0023] Add 50 grams of sodium hydroxide and 250 grams of water into the reaction kettle, then add 30 grams of phenol and 100 grams of methanol into the reaction kettle, and then lower the temperature. 360 grams of methanol solution for dissolving iodine, the methanol solution for dissolving iodine is a mixture of iodine and methyl alcohol with a mass ratio of 1:5, after the dropwise addition, insulated and stirred for 2 hours, and the mass fraction of phenol detected by sampling is less than 3%, Then heat up to 70°C, distill methanol clean, add 129 grams of concentrated hydrochloric acid with a mass fraction of 31% for acidification, keep warm at 45°C for 1 hour, and then cool down to 20°C for centrifugation to obtain a solid crude product. grams of water twice rinse.

[0024] The solid crude product obtained by centrifugation was added to petroleum ether whose mass was 5 times that of the solid crude prod...

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PUM

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Abstract

The invention discloses a p-iodophenol synthesis method, which belongs to the technical field of chemical synthesis, and comprises the following steps: adding sodium hydroxide and water into a reaction kettle, then adding phenol and methanol into the reaction kettle, cooling, dropwise adding a methanol solution for dissolving iodine into the reaction kettle, after dropwise adding, carrying out heat preservation and stirring for 2-2.5 hours, sampling and detecting that the phenol is less than 3%, and determining that the product is qualified; then heating to 70 DEG C, completely distilling methanol, adding concentrated hydrochloric acid for acidification, keeping the temperature at 40-45 DEG C for 1-1.5 hours, cooling to 10-20 DEG C, centrifuging to obtain a solid crude product, and leaching with water during centrifuging; adding a solid crude product obtained by centrifugation into petroleum ether for recrystallization, and performing centrifugal drying to obtain a final white solid product; according to the synthesis method disclosed by the invention, the compound is prepared by adopting a phenol direct iodination process route reaction, the process is simplified, the cost is low, and the yield is high.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis method of p-iodophenol. Background technique [0002] p-iodophenol, also known as 4-iodophenol, is an organic compound with the chemical formula C 6 h 5 IO, as light brown powder. Slightly soluble in water, easily soluble in ethanol, ether and other organic solvents, it can be used as a disinfectant or an intermediate in organic synthesis. At present, the synthesis of p-iodophenol, the drug intermediate of p-iodophenoxyacetic acid, has a long technical process chain and complicated production. Contents of the invention [0003] The technical problem to be solved by this invention is to provide a kind of synthesis method of p-iodophenol. [0004] In order to solve the problems of the technologies described above, the technical scheme adopted in the present invention is as follows: [0005] The method for synthesizing p-iodophenol comprises the followi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/27C07C37/62C07C37/68C07C37/84C07C37/70
Inventor 于广武郭振伟姜春燕杨继军张月
Owner 营口兴福化工有限公司
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