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A kind of synthetic method of guanidine sulfate

A technology for the production of guanidine sulfate and a synthetic method, which is applied in the field of organic drug synthesis, can solve the problems of 1,2-epichlorohydrin's high toxicity, influence on product market competitiveness, and many synthetic steps, and achieve low toxicity and short synthetic route , the effect of simple synthesis steps

Active Publication Date: 2017-07-18
SHANGHAI MODERN HASEN SHANGQIU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned synthesis techniques mostly have the following disadvantages: many synthesis steps, complex operation, low yield, and the toxicity of the raw material 1,2-epichlorohydrin used is relatively high. These factors all affect the market competitiveness of the product and need to be further improved.

Method used

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  • A kind of synthetic method of guanidine sulfate

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Comparison scheme
Effect test

Embodiment 1

[0023] A kind of guanidine sulfate synthetic method, it comprises the steps:

[0024] 1) Synthesis of 2-hydroxymethyl-1,4-benzodioxane:

[0025] Add 20g (182mmol) of ortho-catechol, 80g of water and 39.6g (990mmol) of sodium hydroxide into the reaction bottle, protect it with nitrogen, heat (about 70-80°C) and stir to dissolve, then add 30ml of toluene, stir slowly 29.5 g (200 mmol) of 1,2,3-trichloropropane was added dropwise, and after the dropwise addition was completed, the temperature was raised and refluxed for reaction for 3.5 hours. After the reaction, cool down to below 15°C, separate the organic layer, extract the water layer twice with toluene (20ml*2), combine the toluene layer, wash with water, evaporate the toluene under reduced pressure, add 50ml of water to the residue, heat to dissolve and cool down to 15°C Below ℃, crystals were precipitated, filtered, and dried to obtain 25.0 g of solid 2-hydroxymethyl-1,4-benzodioxane, with a yield of 82%.

[0026] 2) Syn...

Embodiment 2

[0031] A kind of guanidine sulfate synthetic method, it comprises the steps:

[0032] 1) Synthesis of 2-hydroxymethyl-1,4-benzodioxane:

[0033] Add 20g (182mmol) of ortho-catechol, 80g of water and 51g (910mmol) of potassium hydroxide into the reaction bottle, protect with nitrogen, heat (about 70-80°C) and stir to dissolve, then add 30ml of toluene, slowly drop under stirring 29.5 g (200 mmol) of 1,2,3-trichloropropane was added, and after the dropwise addition was completed, the temperature was raised to reflux for 3.5 hours. After the reaction, cool down to below 15°C, separate the organic layer, extract the water layer twice with toluene (20ml*2), combine the toluene layer, wash with water, evaporate the toluene under reduced pressure, add 50ml of water to the residue, heat to dissolve and cool down to 15°C Below ℃, crystals were precipitated, filtered, and dried to obtain 25.7 g of solid 2-hydroxymethyl-1,4-benzodioxane, with a yield of 85%.

[0034] 2) Synthesis of 2-...

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Abstract

The invention belongs to the technical field of organic drug synthesis, and particularly relates to a guanoxan sulfate synthesis method. The method comprises steps as follows: 1), 2-hydroxymethyl-1,4-benzodioxane and thionyl chloride have a chlorination reaction under the condition of existence of a solvent I, and 2-chloromethyl-1,4-benzodioxane is obtained; 2), 2-chloromethyl-1,4-benzodioxane and guanidine are condensed under the condition of existence of alkali and a solvent II, guanoxan is obtained, guanoxan and sulfuric acid are salified, and a finished product guanoxan sulfate is obtained. According to the guanoxan sulfate synthesis method, technological synthesis steps are simple, a route is short, raw material toxicity is relatively lower, and the yield and the purity of the product are high.

Description

technical field [0001] The invention belongs to the technical field of organic medicine synthesis, and in particular relates to a synthesis method of guanidine sulfate. Background technique [0002] Guanidine sulfate, chemical name: 2-guanidinium methyl-1,4-benzodioxane sulfate, also known as guanidine axan, is a powerful antihypertensive drug, the mechanism of action is to prevent norepinephrine Normal release, weakening vasoconstriction, used for essential hypertension, severe and moderate to severe renal and malignant hypertension, this product is white crystalline powder, odorless, soluble in ethanol, soluble in water, insoluble in chloroform and ether. [0003] The synthetic method of the guanidine sulfate that has been reported at present mainly contains: the synthetic method that 470 pages of medical technology compilations are included, or the 5th page of the 4th phase of the 14th volume of Shandong Pharmaceutical Industry Journal in 1995, or the technology reported...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/20
CPCC07D319/20
Inventor 王英利陈洪张颖江正祥刁文瑞刘砺邵冠儒张峰
Owner SHANGHAI MODERN HASEN SHANGQIU PHARMA
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