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Production process of medicinal phloroglucinol

A kind of phloroglucinol, pharmaceutical grade technology, applied in the production technology field of pharmaceutical grade phloroglucinol

Active Publication Date: 2013-04-03
HUNAN ER KANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet the reaction time of this method 1,3,5-trimethoxybenzene and concentrated hydrochloric acid or concentrated sulfuric acid and H3PO4 is long, and easily produces reaction by-products, The obtained phloroglucinol can not meet the requirements of medical phloroglucinol

Method used

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  • Production process of medicinal phloroglucinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 2, the synthesis of phloroglucinol

[0033] 1. Mix 15g of 1,3,5-trimethoxybenzene and 1000ml of 35% concentrated hydrochloric acid into a three-necked flask, add 50ml of H 3 PO 4 , add 0.5g platinum dioxide at the same time, stir at room temperature for 4h, place in ice bath, add 600g Na in batches while stirring 2 CO 3 Neutralize, adjust the pH to 2-3 and then filter. The filtrate was extracted three times with 600ml of methyl tert-butyl ether, the extract was dried over anhydrous sodium sulfate, filtered, and the methyl tert-butyl ether was evaporated to obtain a yellow solid phloroglucinol crude product with a purity of 96.5%. The yield was 86.7%, mp205~210℃.

Embodiment 2

[0034] 2. Take purified water 10 times the amount of the crude product, add crude phloroglucinol, heat to 80°C, stir to dissolve. Add 0.50% activated carbon and keep warm for 45 minutes. The filtrate is firstly filtered through a 0.45 μm filter membrane, and then finely filtered through a 0.22 μm filter membrane to obtain a fine filtrate.

[0035] 3. Pass the finely filtered filtrate through the hollow fiber ultrafiltration membrane. The ultrafiltration membrane adopts a hollow fiber ultrafiltration polysulfone membrane, so that the inlet pressure of the ultrafiltration membrane is controlled at 1.75MPa, and the hollow fiber material line velocity is 1m / s , to obtain the ultrafiltrate.

[0036] 4. Cool the ultrafiltrate to room temperature, crystallize for 4 hours, centrifuge, take the white crystals and dry them in vacuum (-0.085~-0.080MPa, 40~45℃) for 3 hours to obtain pharmaceutical grade phloroglucinol with a purity of 99.9 % (HPLC method).

[0037] Embodiment 3, the synth...

Embodiment 3

[0039] 2. Take purified water 10 times the amount of the crude product, then add the crude product phloroglucinol, heat to 80°C, stir to dissolve. Add 0.50% activated carbon and keep warm for 45 minutes. The filtrate is firstly filtered through a 0.45 μm filter membrane, and then finely filtered through a 0.22 μm filter membrane to obtain a fine filtrate.

[0040] 3. Pass the finely filtered filtrate through the hollow fiber ultrafiltration membrane, the ultrafiltration membrane adopts the hollow fiber ultrafiltration polysulfone membrane, so that the inlet pressure of the ultrafiltration membrane is controlled at 2MPa, and the hollow fiber material line velocity is 1.5m / s , to obtain the ultrafiltrate.

[0041] 4. Cool the ultrafiltrate to room temperature, crystallize for 4 hours, centrifuge, take the white crystals and dry them in vacuum (-0.085~-0.080MPa, 40~45℃) for 3 hours to obtain pharmaceutical grade phloroglucinol with a purity of 99.8 % (HPLC method).

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Abstract

The invention discloses a production process of medicinal phloroglucinol, and belongs to the field of medicine chemical industry. The production process comprises the following steps of: uniformly mixing 1,3,5-trimethoxy benzene with concentrated hydrochloric acid, adding phosphoric acid, and adding a catalyst; stirring for 2-4 hours at room temperature; adding in an ice bath, adding Na2CO3 in different batches while stirring; regulating the pH value to 2-3; filtering; extracting a filtrate for three times by methyl tert-butyl ether; combining the extracting liquids; recovering the methyl tert-butyl ether to obtain a yellow solid, namely coarse phloroglucinol; adding proper amount of pure water into the coarse product to dissolve the coarse product; heating to 80 DEG C, stirring to dissolve the coarse product; adding 0.50% of active carbon, preserving the heat for 45minutes; filtering by a filter membrane of 0.45 microns, and filtering a filtrate by a hollow fiber; and cooling the obtained filtrate to room temperature, crystallizing for 4hours, centrifuging, reserving a white crystal substance, and drying the white crystal substance under a vacuum environment to obtain the product. The production process disclosed by the invention is simple in process, low in cost, high in yield being greater than 85% and high in product purity being greater than 99.8%.

Description

technical field [0001] The invention relates to a production process of pharmaceutical grade phloroglucinol, which belongs to the field of medicine and chemical industry. Background technique [0002] Phloroglucinol, which is 1,3,5-trihydroxybenzene dihydrate, is clinically used as a smooth muscle antispasmodic drug. It can relieve acute spastic pain caused by digestive system and biliary tract dysfunction; acute spastic urethral, ​​bladder, and renal colic; gynecological spastic pain; it can also be used as an adjuvant treatment for uterine contraction during pregnancy. When phloroglucinol is used as a drug, it can be made into sterile powder for injection and orally disintegrating tablets, and it should be avoided to be used in common with morphine and its derivatives because these drugs have spasmogenic effects. [0003] The structural formula of Phloroglucinol is as follows: [0004] [0005] Various synthesis methods of phloroglucinol have been disclosed in the pri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/10C07C37/055
Inventor 帅放文王向峰章家伟
Owner HUNAN ER KANG PHARMA
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