A kind of preparation method of 4-nitrophenyl phosphate sodium salt

A technology of sodium nitrophenyl phosphate and p-nitrophenol, which is applied in the preparation of disodium salt of 4-nitrophenyl phosphate and monosodium salt of 4-nitrophenyl phosphate, which can solve the problem of environment and experimental operators Impact on personal safety, difficulty in meeting the quality requirements of biochemical and diagnostic reagents, and unavoidable pollution of heavy metal barium ions, etc., to achieve the effect of improving product purity, reducing the residue of heavy metal element barium, and simplifying the process implementation process

Active Publication Date: 2011-12-07
广东派特埃尔生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] As we all know, Ba(OH) 2 The price is high, it is uneconomical in production, and the pollution of heavy metal barium ions is inevitable, so it is not suitable for the field of biochemical and diagnostic reagents
At the same time, a large amount of ether is consumed in the extraction process, which causes environmental pollution in addition to poor economic benefits; and the final step of converting to sodium salt uses an aqueous solution environment, which is prone to hydrolysis reactions, resulting in increased impurities in the product, difficult separation, and product color. Turning yellow, it is difficult to meet the quality requirements of biochemical and diagnostic reagents
The use of H in the drying process of the final product 2 SO 4 Vacuum drying, except to consume H 2 SO 4 In addition, it will also have a certain impact on the environment and the personal safety of experimental operators.
[0004] Therefore, there are many defects in the preparation method of pNPP provided in the prior art, and it is not suitable for preparing special fields such as medical diagnostic reagents (IVD) and biochemical reagents.

Method used

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  • A kind of preparation method of 4-nitrophenyl phosphate sodium salt
  • A kind of preparation method of 4-nitrophenyl phosphate sodium salt
  • A kind of preparation method of 4-nitrophenyl phosphate sodium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The process step in the following embodiment 1 is with reference to appendix figure 1 The reaction scheme in .

[0027] 1. Synthesis and separation of intermediate product A:

[0028] Add p-nitrophenol (pNP) and pyridine (Py.) in a molar ratio of 1:6 into a three-necked flask, and stir to dissolve. Then control the temperature at 10-15°C, and after the temperature stabilizes within this range, use a dropper to pour the refined phosphorus oxychloride (POCl 3 ) slowly dropwise into the three-necked flask, after adding one molar equivalent, add an appropriate amount of POCl 3 , to avoid the generation of disubstituted and trisubstituted by-products, and then continue to stir at this temperature for 10 hours to obtain a slurry. At this time, TLC (petroleum ether: ethyl acetate = 1:3) showed that no starting material p-nitrophenol (pNP) remained.

[0029] Suction filter the slurry, the filter cake is washed with toluene, and the obtained filtrate is distilled off under r...

Embodiment 2

[0041] The processing steps in the following embodiment 2 all refer to the appended figure 2 The reaction scheme in .

[0042] 1. Synthesis and separation of intermediate product A:

[0043]Add p-nitrophenol (pNP) and pyridine (Py.) in a molar ratio of 1:8 into a three-neck flask, and stir to dissolve. Then control the temperature at 10-15°C, and after the temperature stabilizes within this range, use a dropper to pour the refined phosphorus oxychloride (POCl 3 ) slowly dropwise into the three-necked flask, after adding one molar equivalent, add an appropriate amount of POCl 3 , to avoid the generation of disubstituted and trisubstituted by-products, and then continue to stir at this temperature for 6-10 hours to obtain a slurry. At this time, TLC (petroleum ether: ethyl acetate = 1:3) showed that no starting material p-nitrophenol (pNP) remained.

[0044] Suction filter the slurry, the filter cake is washed with toluene, and the obtained filtrate is distilled off under r...

Embodiment 3

[0062] 1. Synthesis and separation of intermediate product A:

[0063] Add p-nitrophenol (pNP) and pyridine (Py.) in a molar ratio of 1:2 into a three-necked flask, and stir to dissolve. Then control the temperature at 10-15°C, and after the temperature stabilizes within this range, use a dropper to pour the refined phosphorus oxybromide (POBr 3 ) is slowly added dropwise to the three-necked flask, after adding one molar equivalent, add an appropriate amount of POBr 3 , to avoid the generation of disubstituted and trisubstituted by-products, and then continue to stir at this temperature for 6-10 hours to obtain a slurry. At this time, TLC (petroleum ether: ethyl acetate = 1:3) showed that no starting material p-nitrophenol (pNP) remained.

[0064] Suction filtration slurry, filter cake is washed with toluene, the filtrate decompression distillation that obtains is sloughed off toluene, excessive phosphorus oxybromide (POBr 3 ) and pyridine (Py.) were sealed and stored to pr...

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Abstract

The invention provides a preparation method of 4-nitrophenyl sodium phosphate salts. The preparation method comprises the following steps: treating p-nitrophenol as a raw material; carrying out an addition reaction of p-nitrophenol with POX3; preparing 4-nitrophenyl phosphoric acid through hydrolyzing; preparing 4-nitrophenyl monosodium phosphate salts or 4-nitrophenyl disodium phosphate salts through carrying out a neutralization reaction; and obtaining white powdery finished products through carrying vacuum freeze drying. The preparation method of 4-nitrophenyl sodium phosphate salts provided by the invention allows biochemical reagent graded quality requirements to reached, technological processes to be simple, the cost to be low, the environmental pollution to be reduced, and the product purity to be improved.

Description

【Technical field】 [0001] The invention relates to the technical field of organic synthesis, in particular to the preparation of 4-nitrophenyl phosphate sodium salt, especially 4-nitrophenyl phosphate monosodium salt and 4-nitrophenyl phosphate disodium salt (pNPP) method. 【Background technique】 [0002] pNPP is the abbreviation of organic compound 4-nitrophenyl phosphate disodium salt. Its application involves the fields of biochemical reactions and medical diagnostic reagents, and is a catalytic substrate of alkaline phosphatase. At present, there is no report on the preparation method of pNPP in China, and the only foreign document (THE PREPARATION OFPHENYL PHOSPHORIC ESTERS, BY EARL JUDSON KING AND THOMASFREDERICK NICHOLSON, From the British Postgraduate Medical School, London) provides a method for preparing pNPP. The method is: after p-nitrophenol is prepared into the crude product 4-nitrophenyl phosphoric acid, the barium salt is first prepared, and then the barium s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12
Inventor 钱千里谈宇清
Owner 广东派特埃尔生物科技有限公司
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