Preparation method of phloroglucinol

A technology of phloroglucinol and resorcinol, applied in the field of medicine, can solve the problems of polluted environment, complicated process, low product yield and the like

Inactive Publication Date: 2021-09-10
HAIKOU TIANXINGJIAN PHARMA RES CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The invention provides a preparation method of phloroglucinol, which is used to solve the technical problems of polluting the environment in the existing preparation method of phloroglucinol, complex preparation process, low product yield and yellowish color of the finished product

Method used

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

Examples

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preparation example Construction

[0041] Such as figure 1 Shown, a kind of preparation method of phloroglucinol comprises the steps:

[0042] (1) Get resorcinol in reaction container, add reaction solvent, and reaction solvent comprises any one in chloroform, dichloromethane, acetone, butanone, methyl tert-butyl ether or ether. Stir until dissolved; take N-chlorosuccinimide and add it to the reaction vessel in batches, the molar ratio of N-chlorosuccinimide to resorcinol is 0.8-1.5:1, control the temperature Over 60°C; after the addition, stir and react at 20-60°C for 1 hour, preferably at a reaction temperature of 30-60°C. Then lower the temperature to 10-20° C. and continue stirring for 1 h, filter, wash the filter residue with a pre-cooled reaction solvent, combine the filtrates to obtain a 4-chlororesorcinol solution, and take it out for later use.

[0043] (2) Add potassium hydroxide to the reaction vessel, the molar ratio of potassium hydroxide to 4-chlororesorcinol is 6-20:1. Under the protection of ...

Embodiment 1

[0048] The present embodiment provides a kind of preparation method of phloroglucinol, comprising the following steps:

[0049] (1) Take 110.0g of resorcinol into the reaction vessel, add 440ml of ether, and stir until completely dissolved.

[0050] Take N-chlorosuccinimide and add it to the reaction vessel in 10 batches. The molar ratio of N-chlorosuccinimide to resorcinol is 1.1:1, and the temperature is controlled not to exceed 40°C. After the addition, stir and reflux at 40°C for 1 hour; then lower the temperature to 10-20°C and continue stirring for 1 hour, filter, wash the filter residue with pre-cooled ether, combine the filtrates to obtain 4-chlororesorcinol solution, take it out for later use.

[0051] (2) Take potassium hydroxide into the reaction vessel, the molar ratio of potassium hydroxide to 4-chlororesorcinol is 8:1. Under the protection of nitrogen, heat the potassium hydroxide in an environment of 145° C. to melt, then add the 4-chlororesorcinol solution pre...

Embodiment 2

[0056] The present embodiment provides a kind of preparation method of phloroglucinol, comprising the following steps:

[0057] (1) Take 110.0 g of resorcinol into a reaction vessel, add 330 ml of reaction solvent methyl tert-butyl ether, and stir until completely dissolved.

[0058] Take N-chlorosuccinimide and add it to the reaction vessel in 10 batches, the molar ratio of N-chlorosuccinimide to resorcinol is 1:1, and the temperature is controlled not to exceed 50°C. After the addition, stir and react at 45°C for 1h; then lower the temperature to 10-20°C and continue stirring for 1h, filter, wash the filter residue with pre-cooled methyl tert-butyl ether, and combine the filtrates to obtain 4-chlororesorcinol solution , 4-chlororesorcinol content determination high performance liquid chromatogram is as figure 2 shown.

[0059] (2) Take potassium hydroxide into the reaction vessel, the molar ratio of potassium hydroxide to 4-chlororesorcinol is 10:1. Under the protection ...

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Abstract

The invention discloses a preparation method of phloroglucinol, which comprises the following steps: chloridizing a starting material resorcinol by using N-chlorosuccinimide to obtain an intermediate 4-chlororesorcinol, and reacting the intermediate 4-chlororesorcinol with potassium hydroxide to obtain phloroglucinol. The synthesis method has the advantages of few reaction steps, mild reaction conditions and safety in operation, and compared with the existing preparation method, the production cost is lower, and the amount of generated high-pollution wastes is less. The invention also provides a novel synthesis method of the intermediate 4-chlororesorcinol, and through optimization, the whole reaction process avoids using toxic solvents, and meanwhile, the problem that a phloroglucinol finished product becomes yellow is well solved.

Description

technical field [0001] The invention belongs to the technical field of medicine, in particular to a preparation method of phloroglucinol. Background technique [0002] Phloroglucinol is a myophilic non-atropine non-papaverine pure smooth muscle antispasmodic, which can directly act on the smooth muscle of the gastrointestinal tract and genitourinary tract, and is superior to a wide range of anticholinergic antispasmodics. Phloroglucinol has the advantages of fast antispasmodic and analgesic effect, high safety factor and no toxic and side effects. It will not produce a series of anticholinergic side effects, and will not cause symptoms such as hypotension, increased heart rate, and arrhythmia. Vascular function is not affected, mainly used for the treatment of acute spasmodic pain caused by digestive system and biliary tract dysfunction, acute spasmodic urethra, bladder, renal colic and gynecological spasmodic pain. [0003] Phloroglucinol exists in many natural plants in t...

Claims

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Application Information

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IPC IPC(8): C07C37/02C07C37/82C07C37/84C07C39/10C07C37/62C07C39/24
CPCC07C37/02C07C37/82C07C37/84C07C37/62C07C39/245C07C39/10
Inventor 陈恳凌秀才李庆明肖茂锐尹朝亮黄敢行
Owner HAIKOU TIANXINGJIAN PHARMA RES CO LTD
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