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Iopamidol synthesis and preparation of iopamidol synthesis intermediate

A technology of iopamidol and intermediates is applied in the field of synthesis and the preparation of synthetic intermediates, can solve the problems of waste of reactants, difficult production and the like, and achieves the effects of less reaction time, production cost saving, and fast reaction rate

Inactive Publication Date: 2019-02-01
HUBEI TIANSHU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the disadvantages of being difficult to produce and waste of reactants in the prior art, and propose a synthesis of iopamidol and the preparation of its synthetic intermediate

Method used

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  • Iopamidol synthesis and preparation of iopamidol synthesis intermediate
  • Iopamidol synthesis and preparation of iopamidol synthesis intermediate
  • Iopamidol synthesis and preparation of iopamidol synthesis intermediate

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preparation example Construction

[0030] A kind of synthesis of iopamidol and the preparation of synthetic intermediate thereof, the synthesis of described iopamidol and the preparation technology of synthetic intermediate thereof comprise following route and step:

[0031] The molecular structure of described iopamidol is as shown in formula 1:

[0032]

[0033] The preparation process route is as follows:

[0034]

[0035]

[0036] Step 1: Mix a certain amount of compound A and iodine chloride in a reaction vessel, add a certain amount of catalyst, and react fully to generate compound B, hydrogen chloride and water;

[0037] Step 2: Take a certain amount of compound B and phosphorus pentachloride and mix them in a reaction vessel. After fully reacting, compound C is generated;

[0038] Step 3: Mix a certain amount of compound C and acetoxy compound in a reaction vessel, add a certain amount of catalyst, and react fully to generate compound D and water;

[0039] Step 4: Mix a certain amount of comp...

Embodiment

[0043] S1: Mix 200g of compound A and 300g of iodine chloride in a container, and then continue to pour hydrogen into the container to control the intake rate of hydrogen, and control the total molar amount of hydrogen to 20 moles until the end of the reaction , the reaction temperature is controlled at about 70 degrees Celsius, and the reaction time is controlled at 5 hours. During the reaction, the conduit is connected to the exhaust port of the reaction vessel, and the other end of the conduit is connected to a sealed collection container;

[0044] S2: adding a certain amount of hydrochloric acid to the mixed solution after the reaction of compound A and iodine chloride, so that the pH value of the mixed solution is about 5;

[0045] S3: in step 1, the product generated after the reaction of compound A and iodine chloride is compound B, get 100g compound B and 150g phosphorus pentachloride and mix in a container, the reaction temperature is controlled at about 30 degrees Cel...

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Abstract

The invention relates to the technical field of chemical synthesis processes, particularly to iopamidol synthesis and preparation of an iopamidol synthesis intermediate. According to the present invention, by adjusting the feeding weight ratio, optimizing the reaction conditions and improving the iopamidol synthesis route, the requirements on the compound reaction conditions are low, the control of the reaction is simple, and the yield is increased while the quality of the intermediate product is greatly improved so as to reduce the process control difficulty in the iopamidol production process and improve the quality and the qualification rate of iopamidol; and various steps of the preparation process are simple, the solvents and the process conditions are safe and easy to perform, the environmental protection production is achieved, and the method has broad application prospects.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis technology, in particular to a synthesis of iopamidol and the preparation of a synthesis intermediate thereof. Background technique [0002] Iopamidol is a drug with the chemical name (S)-N,N-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-[(2-hydroxy-1-oxypropyl) Amino]-2,4,6-triiodo-1,3-benzenedicarboxamide, iopamidol is a non-ionic water-soluble contrast agent, because of its high iodine content, it attenuates X-rays to achieve contrast imaging Purpose, suitable for X-ray angiography for intravascular injection. Clinically, iopamidol is used for various angiography, such as cerebral angiography, cardiovascular angiography, etc. At present, there are many routes for synthesizing iopamidol, for example, WO9705097A1WO2012007547A1 It was reported that 5-hydroxy-2,4,6-triiodo-1,3-benzenedicarboxylic acid was amidated with 2-amino-1,3-propanediol, and then derivatized with (R)-2-propionamide rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/46C07C231/02C07C231/12C07C235/16C07C229/62C07C227/04C07C227/02
CPCC07C227/02C07C227/04C07C229/62C07C231/02C07C231/12C07C235/16C07C237/46
Inventor 刘云龙
Owner HUBEI TIANSHU PHARMA CO LTD
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