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Preparing technology of 3-(N-morpholino)-2-hydroxypropanesodium sulfonate

A kind of sodium hydroxypropanesulfonate and a preparation technology, applied in the field of preparation technology of 3--2-hydroxypropanesulfonate sodium, can solve the problems of low yield, achieve high preparation efficiency, low production cost, and improve preparation efficiency Effect

Inactive Publication Date: 2016-10-12
SUQIAN YUANYANG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation technology of 3-(N-morpholine)-2-hydroxypropanesulfonate sodium has the problem of low yield

Method used

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  • Preparing technology of 3-(N-morpholino)-2-hydroxypropanesodium sulfonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of preparation technology of 3-(N-morpholine)-2-hydroxy propanesulfonate sodium, comprises the steps:

[0025] (1) Synthesis of 3-(N-morpholine) ionic liquid

[0026] First, morpholine and acid are mixed at a molar ratio of 1:1, stirred and reacted for 6 hours at a reaction temperature of -10°C and in an inert gas, washed, and then subjected to reduced-pressure distillation to obtain a liquid for use. The acid is hydrochloric acid, Hydrobromic acid and trifluoromethanesulfonic acid, the morpholine and the acid are mixed in a solvent, the solvent is N,N-dimethylformamide, and the inert gas is nitrogen;

[0027] (2) Synthesis of 3-(N-morpholine) sodium salt

[0028] React the obtained 3-(N-morpholine) ionic liquid with sodium bisulfite, ionized water and a catalyst, raise the temperature to 80° C., and keep it warm for 1 hour to obtain 3-(N-morpholine) sodium salt;

[0029] (3) Synthesis of 3-(N-morpholine) sodium propanesulfonate

[0030] When the obtained 3-(N...

Embodiment 2

[0036] A kind of preparation technology of 3-(N-morpholine)-2-hydroxy propanesulfonate sodium, comprises the steps:

[0037] (1) Synthesis of 3-(N-morpholine) ionic liquid

[0038] First, morpholine and acid are mixed at a molar ratio of 3:1, stirred and reacted for 27 hours at a reaction temperature of 35°C and in an inert gas, washed, and then subjected to vacuum distillation to obtain a liquid for use. The acid is hydrochloric acid, hydrogen Iodic acid and methanesulfonic acid, the morpholine and the acid are mixed in a solvent, the solvent is N,N-dimethylacetamide, and the inert gas is nitrogen;

[0039] (2) Synthesis of 3-(N-morpholine) sodium salt

[0040] The obtained 3-(N-morpholine) ionic liquid was reacted with sodium bisulfite, ionized water and a catalyst, the temperature was raised to 85° C., and kept for 1.5 h to obtain 3-(N-morpholine) sodium salt;

[0041] (3) Synthesis of 3-(N-morpholine) sodium propanesulfonate

[0042] When the obtained 3-(N-morpholine) s...

Embodiment 3

[0048] A kind of preparation technology of 3-(N-morpholine)-2-hydroxy propanesulfonate sodium, comprises the steps:

[0049] (1) Synthesis of 3-(N-morpholine) ionic liquid

[0050] First, morpholine and acid are mixed at a molar ratio of 5:1, stirred and reacted for 48 hours at a reaction temperature of 80° C. and in an inert gas, washed, and then subjected to vacuum distillation to obtain a liquid for use. The acid is methylsulfonate Acid, p-toluenesulfonic acid and trifluoromethanesulfonic acid, the morpholine and the acid are mixed in a solvent, the solvent is dimethyl sulfoxide, and the inert gas is helium;

[0051] (2) Synthesis of 3-(N-morpholine) sodium salt

[0052] React the obtained 3-(N-morpholine) ionic liquid with sodium bisulfite, ionized water and a catalyst, raise the temperature to 90°C, and keep it warm for 2 hours to obtain 3-(N-morpholine) sodium salt;

[0053] (3) Synthesis of 3-(N-morpholine) sodium propanesulfonate

[0054] When the obtained 3-(N-morpho...

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Abstract

The invention discloses a preparing technology of 3-(N-morpholino)-2-hydroxypropanesodium sulfonate. Morpholine and acid are mixed in a solvent, the solvent provides reaction atmosphere, mixing of the morpholine and the acid is promoted, the content of the 3-(N-morpholino) sodium propanesulfonate in reaction liquid can be improved through an ion exchange reaction, and therefore preparing efficiency is improved; due to the proportion of the 3-(N-morpholino) sodium propanesulfonate to a positioning agent, the product can have good purity and good preparing efficiency; due to a ventilation terminal point, the production cost can be reduced while it is determined that the reaction is completed. The 3-(N-morpholino)-2-hydroxypropanesodium sulfonate prepared with the preparing technology has the advantages of being low in production cost and high in preparing efficiency, market potential is huge, and prospects are broad.

Description

technical field [0001] The invention belongs to the preparation field of 3-(N-morpholine)-2-hydroxypropanesulfonate sodium, more specifically, the present invention relates to a kind of 3-(N-morpholine)-2-hydroxypropanesulfonate sodium Preparation Process. Background technique [0002] Sodium 3-(N-morpholino)-2-hydroxypropanesulfonate is a chemical with a molecular weight of 247.20. The English name is 3-(N-Morpholino)-2-hydroxypropanesulfonic acid, Sodium Salt. The quality specifications are purity: ≥99.0%; loss on drying: <0.5%; insoluble matter: <0.1%; chloride (Cl): <0.05%; heavy metal (Pb): <0.0005%. The current preparation technology of 3-(N-morpholine)-2-hydroxypropanesulfonate sodium has the problem of low yield. Contents of the invention [0003] The problem to be solved by the present invention is to provide a preparation process of 3-(N-morpholine)-2-hydroxypropanesulfonate sodium. [0004] In order to achieve the above object, the technical sche...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/088
CPCC07D295/088
Inventor 袁雪生
Owner SUQIAN YUANYANG BIOTECH