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A kind of preparation method of high-purity sodium picosulfate

A sodium picosulfate and high-purity technology, which is applied in the field of preparation of high-purity sodium picosulfate, can solve the problems of low methane purity, complicated operation, and difficult to obtain raw materials, so as to achieve cheap and easy raw materials, reduce environmental pollution, The effect of saving resources

Active Publication Date: 2017-09-22
SHANDONG LUOXIN PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Thereby the 4,4'-dihydroxyphenyl-(2-pyridine) methane purity that prepares is not high, affects the purity of final product sodium picosulfate
[0007] US2827465 discloses a synthetic method to avoid the generation of ortho isomers, using 4', 4"-dimethoxydiphenylacetonitrile and 2-bromopyridine as raw materials to obtain 4', 4"- Dimethoxydiphenyl-(2-pyridine)-acetonitrile, add 48% hydrobromic acid to reflux reaction, hydrolyze the cyano group and remove the methyl group simultaneously, obtain 4', 4"-dihydroxydiphenyl-( 2-pyridine)-acetamide, then heated to reflux in potassium carbonate aqueous solution to obtain 4', 4 "-dihydroxydiphenyl-(2-pyridine)-methane. Suitable for industrial production

Method used

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  • A kind of preparation method of high-purity sodium picosulfate

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Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1: 4 ', 4 " the synthesis of-dihydroxydiphenyl-(2-pyridine)-methane (compound 4)

[0029] In a 250ml three-neck flask, add 32g of 98% concentrated sulfuric acid at 0-5°C, stir and add 28.2g of phenol, stir for 2 hours, add 10.7g of 2-pyridinecarbaldehyde dropwise at 5-15°C, drop for 0.5-1 hour After the addition is complete, stir and react at room temperature for 1 hour; cool in an ice bath, add 50ml of water at 0-10°C, stir for 10 minutes, adjust the pH value to 7 with 2mol / L sodium hydroxide solution, and filter with suction to obtain a light yellow solid .

[0030] The filtrate obtained by filtration was adjusted to pH 1 with sulfuric acid, stirred for 0.5 hours, added 100 ml of ethyl acetate and extracted three times, combined the organic phases, concentrated, dried over anhydrous sodium sulfate, and recovered phenol was obtained.

[0031] Dissolve the light yellow solid with water / tetrahydrofuran at a volume ratio of 2:1, adjust the pH to 8.0 with 1mol / ...

Embodiment 2

[0033] Embodiment 2: 4 ', 4 " the synthesis of-dihydroxydiphenyl-(2-pyridine)-methane (compound 4)

[0034] In a 250ml three-neck flask, add 28g of 98% concentrated sulfuric acid at 0-5°C, stir and add 23.5g of phenol, stir for 2 hours, add 10.7g of 2-pyridinecarbaldehyde dropwise at 5-15°C, drop for 0.5-1 hour After the addition is complete, stir and react at room temperature for 1 hour; cool in an ice bath, add 50ml of water at 0-10°C, stir for 10 minutes, adjust the pH value to 7 with 2mol / L sodium hydroxide solution, and filter with suction to obtain a light yellow solid .

[0035] Dissolve the light yellow solid with water / tetrahydrofuran with a volume ratio of 3:1, adjust the pH to 8.2 with 1mol / L sodium hydroxide, then add ferrous ammonium sulfate until the solution is light blue, and heat to 40-50 ℃, the color does not disappear; then adjust the pH value to 6.5-7.0 with sulfuric acid, a large amount of solid precipitates, filter with suction, and wash the filter cake ...

Embodiment 3

[0036] Embodiment 3: 4 ', 4 " the synthesis of-dihydroxydiphenyl-(2-pyridine)-methane (compound 4)

[0037] In a 250ml three-neck flask, add 37.5g of 98% concentrated sulfuric acid at 0-5°C, stir and add 33g of phenol, stir for 2 hours, add 10.7g of 2-pyridinecarbaldehyde dropwise at 5-15°C, drop for 0.5-1 hour After the addition is complete, stir and react at room temperature for 1 hour; cool in an ice bath, add 50ml of water at 0-10°C, stir for 10 minutes, adjust the pH value to 7 with 2mol / L sodium hydroxide solution, and filter with suction to obtain a light yellow solid .

[0038] Dissolve the light yellow solid with water / tetrahydrofuran at a volume ratio of 2.5:1, adjust the pH to 8.4 with 1mol / L sodium hydroxide, then add ferrous ammonium sulfate until the solution is light blue, and heat to 40-50 ℃, the color does not disappear; then adjust the pH value to 6.5-7.0 with sulfuric acid, a large amount of solid precipitates, filter with suction, and wash the filter cake ...

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Abstract

The invention belongs to the field of medicine chemical engineering, particularly to a method for preparing high-purity sodium picosulfate. The method mainly comprises the following steps: condensing 2-pyridylaldehyde (a compound 2) and phenol (a compound 3) to obtain 4',4''-dihydroxy diphenyl-(2-pyridine)-methane (a compound 4) and ortho-isomeride 2',4''-dihydroxy diphenyl-(2-pyridine)-methane (a compound 5), dissolving the compound 4 and the compound 5 with water / furanidine, adjusting the pH to 8.0-8.5, adding ammonium ferrous sulfate until the solution is light blue, then adjusting the pH value to 6.5-7.0, dissolving out plenty of solid, conducting suction filtration to separate the high purity compound 4, and further synthesizing sodium picosulfate.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a preparation method of high-purity sodium picosulfate. Background technique [0002] Sodium picosulfate, also known as sodium picosulfate, chemical name: 4,4'-(pyridin-2-ylmethylene) bisphenyl bissulfate sodium, is a laxative developed by Italian company De Angeli, it is A special laxative with a unique mode of action, which directly acts on the large intestine mucosa to produce a mild laxative effect. It can not only be used for various forms of constipation, but also relieve pain caused by hemorrhoids or anal fissures. It is also used for defecation difficulty. [0003] In addition, on July 16, 2012, the FDA approved Sodium Picosulfate-Magnesium Oxide-Citrate (trade name: Prepopik) oral powder from Ferring Pharmaceuticals, Switzerland, to be used for colon cleansing before colonoscopy in adults. Not listed in our country yet. [0004] Swiss patent 1...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/30
CPCC07D213/30
Inventor 陈雨王瑞杨林林
Owner SHANDONG LUOXIN PHARMA GRP CO LTD
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