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Preparation method of phloroglucinol

A technology of phloroglucinol and dichlorophenol, which is applied in the field of preparation of phloroglucinol, can solve problems such as inability to realize industrialized production, consume a large amount of solvent, and difficult sources of raw materials, and achieve reduced processing difficulty, less solvent loss, Easy to prepare

Active Publication Date: 2013-05-08
JIANGSU DINGYE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the reaction process of this route is simple, there is no good synthetic method for 2,4- or 2,6-dihydroxychlorobenzene at present, so the cost of raw materials is high and the source is difficult
Simultaneously in the reaction process, there is also the problem of waste acid treatment, and in the separation and purification of the final product, the process is complex, the amount of solvent consumed is very large, and the cost of the product is relatively high; (5) benzene triester derivative method
Using benzenetriester derivatives as raw materials, the reaction is complex and the source of raw materials is difficult
It is only suitable for a small amount of preparation in the laboratory, and it is not yet possible to realize industrial production
Simultaneously, a large amount of by-products are produced in the reaction process, the environmental pollution is serious, the yield of the product is relatively low, and separation and purification are difficult; (6) dichlorophenol method

Method used

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  • Preparation method of phloroglucinol
  • Preparation method of phloroglucinol
  • Preparation method of phloroglucinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a 2000mL four-neck flask, add 1.0mol (163.0g) 2,6-dichlorophenol, 8.0mol (448.8g) potassium hydroxide, 0.163g cuprous chloride, 815.0g (930.6mL) 1,2, 4-Trimethylbenzene, heat and keep the bath temperature at 170°C, mix and stir for 17 hours, transfer to a separatory funnel after cooling to room temperature, add 652.0g of water, stand to separate layers, separate the upper solvent, the lower layer The water phase is adjusted to a pH of 0.5 with 37% hydrochloric acid by mass percentage, and the acid water is separated by centrifugation. The crude phloroglucinol is dissolved in hot water, decolorized by activated carbon, and centrifuged to separate the waste activated carbon. The mother liquor is recrystallized, centrifuged, and separated. The mother liquor is produced, and the refined product is dried and pulverized to obtain the finished product with a yield of 68%.

Embodiment 2

[0023] In a 2000mL four-necked flask, add 1.0mol (163.0g) 2,6-dichlorophenol, 9.0mol (504.9g) potassium hydroxide, 1.63g copper sulfate, 978.0g (1116.7mL) 1,2,4- Trimethylbenzene, heating and keeping the bath temperature at 180 °C, mixed and stirred for 14 hours, cooled to room temperature, transferred to a separatory funnel, added 815.0 g of water, allowed to stand for layers, separated the upper solvent, and the lower water phase The pH was adjusted to 3.0 with 31% hydrochloric acid by mass percentage, and the remaining steps were the same as in Example 1, and the yield was 71%.

Embodiment 3

[0025] In a 2000mL four-neck flask, add 1.0mol (163.0g) 2,6-dichlorophenol, 8.5mol (476.9g) potassium hydroxide, 0.83g cuprous chloride, 896.5g (1023.5mL) 1,2, 4-Trimethylbenzene, heat and keep the bath temperature at 175°C, mix and stir for 15 hours, transfer to a separatory funnel after cooling to room temperature, add 733.5g of water, stand to separate layers, separate the upper solvent, the lower layer The pH of the aqueous phase was adjusted to 1.5 with 35% hydrochloric acid by mass percentage, and the rest of the steps were the same as in Example 1, and the yield was 69%.

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Abstract

The invention discloses a preparation method of phloroglucinol, which is implemented by taking 2, 6-dichlorophenol and potassium hydroxide as raw materials and taking 1, 2, 4-trimethylbenzene as a solvent through heating the raw materials and the solvent at normal pressure under the catalysis of copper salt. The method disclosed by the invention has the advantages that (1) phloroglucinol is wide in raw material sources and convenient to prepare; and a catalyst is high in activity and less in application amount; (2) due to normal-pressure reaction, the loss of the solvent is few, and water is added when the reaction is completed, an organic solvent is separated from a liquid phase, and an aqueous phase is subjected to the next step reaction, so that the working procedures that the organic solvent participates in the reaction are reduced, and the technological process is reduced; and (3) the post-reaction treatment is convenient, and the yield is high.

Description

a technical field [0001] The invention relates to a preparation method of phloroglucinol, which belongs to the technical field of chemical material preparation. This method is applicable to the occasion of synthesizing phloroglucinol with dichlorophenol as raw material. Two background technology [0002] Phloroglucinol (1,3,5-trihydroxybenzene) is an important fine chemical product, mainly used in the synthesis of flavonoid isoflavone antitumor drugs, and can also be used as dye coupler, tire tackifier and Azo composite ink and other raw materials; it is used in textile and leather dyeing process, production of plastic capsules, replacement of silver iodide for artificial rainfall, and preservative of some synthetic materials. Phloroglucinol injection can be used for acute spastic pain caused by digestive system and biliary tract dysfunction, acute spastic urethra, bladder, renal colic and gynecological spastic pain. [0003] Currently, there are two types of methods for p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/10C07C37/02
Inventor 戴长喜周永广
Owner JIANGSU DINGYE PHARMA CO LTD
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