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Method for preparing 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 reduce environmental pollution, and the raw materials are cheap and easy to obtain, The effect of saving resources

Active Publication Date: 2016-02-03
SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK 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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  • Method for preparing high-purity sodium picosulfate

Examples

Experimental program
Comparison scheme
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, and complete the dropwise addition in 0.5-1 hour , stirred and reacted at room temperature for 1 hour; cooled in an ice bath, added 50ml of water at 0-10°C, stirred for 10 minutes, adjusted the pH value to 7 with 2mol / L sodium hydroxide solution, and filtered 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...

Embodiment 2

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

[0034] In a 250ml three-necked 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, and complete the dropwise addition in 0.5-1 hour , stirred and reacted at room temperature for 1 hour; cooled in an ice bath, added 50ml of water at 0-10°C, stirred for 10 minutes, adjusted the pH value to 7 with 2mol / L sodium hydroxide solution, and filtered 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 t...

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, and complete the dropwise addition in 0.5-1 hour , stirred and reacted at room temperature for 1 hour; cooled in an ice bath, added 50ml of water at 0-10°C, stirred for 10 minutes, adjusted the pH value to 7 with 2mol / L sodium hydroxide solution, and filtered 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...

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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 DeAngeli company in Italy. It is a 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 in defecation caused by hemorrhoids or anal fissures, and it can also be used for difficult defecation . [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. ...

Claims

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Application Information

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IPC IPC(8): C07D213/30
CPCC07D213/30
Inventor 陈雨王瑞杨林林
Owner SHANDONG LUOXIN PARMACEUTICAL GROUP STOCK CO LTD