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Method for preparing and refining 1,3-propanedisulfonate

A kind of technology of sodium propanedisulfonate and purification method, which is applied in the field of preparation and purification of 1,3-sodium propanedisulfonate, and achieves the effects of low cost, high yield and short reaction time

Inactive Publication Date: 2011-04-06
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are serious defects in this method: 1. In order to remove excess sodium sulfite and bromide ions, precious metal compounds such as silver nitrate, lead acetate and barium hydroxide are repeatedly used in this process. Not only the production cost is high, but also there are many "three wastes" and serious pollution
2. This process requires at least four recrystallizations to obtain qualified sodium 1,3-propanedisulfonate, and the yield is only 30-50%, which is obviously low
3. The raw materials used in this process are 1,3-dibromopropane, silver nitrate, lead acetate and barium hydroxide, which are all expensive and not suitable for industrial production
4. The operation is cumbersome, time-consuming and labor-intensive
[0009] This route 1,3-propanediane sultone is expensive, which is several times that of the raw material 1,3-dichloropropane used in the present invention, and the process is not economical ;In addition, 1,3-propanediane sultone is unstable and easily hydrolyzed, which brings potential harmful impurities to the product:

Method used

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  • Method for preparing and refining 1,3-propanedisulfonate

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Add 150 g of deionized water and 11.3 g (0.10 mol) of 1,3-dichloropropane into the reaction flask, stir, and add 25.2 g (0.20 mol) of anhydrous sodium sulfite for 8 hours. Cool to room temperature, add 300ml of absolute ethanol, stir for 30min, let stand for 2hr, filter with suction, wash the filter cake with a small amount of ethanol, and dry in vacuum to obtain 23.6g of crude sodium 1,3-propanedisulfonate (white solid), The content is 95.6%.

Embodiment 2

[0042] Add 150 g of deionized water and 11.3 g (0.10 mol) of 1,3-dichloropropane into the reaction flask, stir, add 30.3 g (0.24 mol) of anhydrous sodium sulfite, and reflux for 8 hours. Cool to room temperature, add 250ml of absolute ethanol, stir for 30min, let stand for 2hr, filter with suction, wash the filter cake with a small amount of ethanol, and dry it in vacuum to obtain crude sodium 1,3-propanedisulfonate, yield 22.4g, content 89.3%.

Embodiment 3

[0044] Add 150 g of deionized water and 11.3 g (0.10 mol) of 1,3-dichloropropane into the reaction flask, stir, add 20.1 g (0.16 mol) of anhydrous sodium sulfite, and reflux for 8 hours. Cool to room temperature, add 400ml of absolute ethanol, stir for 30min, let stand for 2hr, filter with suction, wash the filter cake with a small amount of ethanol, and dry in vacuum to obtain 20.4 crude sodium 1,3-propanedisulfonate with a content of 97.2%.

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Abstract

The invention relates to a method for preparing and refining 1,3-propanedisulfonate and aims to solve technical problems of raw material cost reduction, stability, process simplification and product yield improvement. The preparation method is to react 1,3-dichloropropane and sodium sulfite in a reaction solvent to obtain coarse 1,3-propanedisulfonate, wherein the mole ratio of the 1,3-dichloropropane to the sodium sulfite is 1:1-4. The refining method is to dissolve the coarse 1,3-propanedisulfonate in water, add crystallizing agent, namely an organic solvent which can be mixed with water, to obtain 1,3-propanedisulfonate, wherein the amount of water is 2 to 20 times the weight of the coarse 1,3-propanedisulfonate.

Description

[0001] technical field [0002] The invention relates to the field of pharmaceutical chemical synthesis, in particular to a method for preparing and refining sodium 1,3-propanedisulfonate. Background of the invention [0003] US Patent US5643562 discloses that 1,3-propanedisulfonate can be used to treat amyloidosis, and world patent WO2007125385 discloses that 1,3-propanedisulfonate can also be used to treat nephropathy, diabetic nephropathy and dyslipidemia. In fact, abroad, sodium 1,3-propanedisulfonate has entered phase III clinical trials for the treatment of amyloidosis, and phase II clinical trials for the treatment of diabetes. Will be available for sale soon. [0004] The synthesis of 1,3-propanedisulfonate sodium was reported as early as the 1930s, and the literature [J.Am.Chem.Soc.1936; 58: 488-9] synthesized 1,3-propanedisulfonate sodium is to react 1,3-dibromopropane with sodium sulfite: [0005] [0006] Repeated treatment with lead acetate, silver nitrate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/05C07C303/32C07C303/44
Inventor 金春华张华星程花英
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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