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A kind of synthetic method of morpholine amididine hydrochloride

A technology for the synthesis of morpholine amididine hydrochloride and its synthesis method, which is applied in the field of synthesis of morpholine amididine hydrochloride, can solve the problems of difficult industrial application, large hydrogen peroxide oxidation heat release, and low yield, and achieve less waste liquid discharge and environmental protection , the effect of reducing the reaction temperature

Active Publication Date: 2017-07-21
NINGXIA SIKEDA BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This solution is difficult to apply industrially due to the large heat release and low yield of hydrogen peroxide oxidation.

Method used

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  • A kind of synthetic method of morpholine amididine hydrochloride
  • A kind of synthetic method of morpholine amididine hydrochloride
  • A kind of synthetic method of morpholine amididine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0039] (1) add diethylene glycol 2.1Kg, dicyandiamide 2.0Kg, ammonium chloride 1.4Kg successively in the reactor of 10L band mechanical stirrer, mass mass concentration is the sulfuric acid aqueous solution 0.5Kg of 30%, under sealed stirring state , the temperature was raised to 120°C at a rate of 3°C per minute, the pressure of the reactor was raised to 0.3MPa, and after 1 hour of reaction, the reaction temperature was naturally cooled to room temperature to obtain a white emulsion;

[0040](2) Transfer the white emulsion to a 50L glass reactor, add 15Kg of 95% ethanol, heat and reflux for 30 minutes to obtain a mixed solution, heat the mixed solution through a filter cartridge to a crystallization kettle, and cool the filtrate in a crystallization kettle After reaching room temperature, white crystals were precipitated, and after centrifugation, they were dried in a hot air oven at 80°C to obtain 5.2Kg of morpholine amididine hydrochloride, with a yield of 81% based on dicya...

Embodiment 2

[0042] (1) add diethylene glycol 3.1Kg, dicyandiamide 3.0Kg, ammonium chloride 2.0Kg successively in the reactor of 10L band mechanical stirrer, mass concentration is the aqueous solution 0.5Kg of 20% sulfuric acid, under sealed stirring state, Raise the temperature to 120°C at a rate of 3°C per minute, and raise the pressure of the reactor to 0.5MPa. After reacting for 1 hour, naturally cool the reaction temperature to room temperature to obtain a white milky product;

[0043] (2) Transfer the white emulsion to a 50L glass reaction kettle, add 28Kg of 95% ethanol, heat and reflux for 30 minutes to obtain a mixed solution, heat the mixed solution through a filter cartridge to a crystallization kettle, and cool the filtrate in a crystallization kettle After reaching room temperature, white crystals were precipitated, and after centrifugation, they were dried in a hot air oven at 85°C to obtain 6.2Kg of morpholine amididine hydrochloride, with a yield of 83% based on dicyandiamid...

Embodiment 3

[0045] (1) add diethylene glycol 2.6Kg, dicyandiamide 2.5Kg, ammonium chloride 1.6Kg successively in the reactor of 10L band mechanical stirrer, mass concentration is 0.5Kg of aqueous sulfuric acid solution of 20%, under sealed stirring state, Raise the temperature to 130°C at a rate of 5°C per minute, and raise the pressure of the reactor to 0.4MPa. After reacting for 1 hour, naturally cool the reaction temperature to room temperature to obtain a white milky product;

[0046] (2) Transfer the white emulsion to a 50L glass reaction kettle, add 20Kg of 95% ethanol, heat and reflux for 30 minutes to obtain a mixed solution, heat the mixed solution through a filter cartridge to a crystallization kettle, and cool the filtrate in a crystallization kettle After reaching room temperature, white crystals were precipitated. After centrifugation, they were dried in a hot air oven at 80° C. to obtain 5.3 kg of morpholine amididine hydrochloride, with a yield of 85% based on dicyandiamide....

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Abstract

The invention discloses a synthetic method of moroxydine hydrochlofide. The method comprises the following steps: adding diglycol, dicyandiamide, ammonium chloride and an aqueous sulfuric acid solution with the mass concentration of 20-30% to a high pressure reaction kettle according to amass ratio of (4-6):(4-6):(2-4):(1-2), heating the obtained solution in a sealed and stirring state to 120-130DEG C, reacting under a reaction kettle pressure of 0.3-0.5MPa for 1-2h, and cooling the obtained solution to room temperature to obtain a white milk; and transferring the white milk to a reaction kettle, adding 95% ethanol according to a volume ratio of the 95% ethanol to diglycol of (7-9):1, carrying out a heating refluxing reaction for 30min to obtain a mixed solution, carrying out hot filtration on the mixed solution through a filter cylinder to a crystallization kettle, cooling the obtained filtrate in the crystallization kettle to room temperature to precipitate white crystals, centrifuging and separating the white crystals, and drying the separated white crystals in a hot wind oven at 80-85DEG C to obtain moroxydine hydrochlofide.. Moroxydine hydrochlofide is obtained through a direct reaction of dicyandiamide and morpholine hydrochloride generated through in situ reaction of diglycol and ammonium chloride under the action of sulfuric acid, so the synthetic method is simplified, side reactions are reduced, the yield is improved, and environment is protected.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing morpholine amididine hydrochloride. Background technique [0002] Morpholine guanidine, also known as morpholine guanidine, commonly known as "viral spirit", as an antiviral chemical raw material drug, can inhibit the reproduction of certain viruses in cells. It is mainly used for the prevention and treatment of viral influenza, mumps, chickenpox, herpes zoster, herpetic stomatitis and other viral diseases. It can also be used in animal husbandry, aquatic products and pesticide industries. It has a wide range of uses. When used as a drug, the compound is usually produced in the form of morpholine amidine hydrochloride, which can inhibit the reproduction of viruses by inhibiting the synthesis of DNA and RNA polymerases of certain viruses in cells, including influenza A H1N1, influenza virus, para Influenza virus, coronavirus, rhinovirus, adenovirus, etc....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/215
CPCC07D295/215
Inventor 田永富陈红余孙风程
Owner NINGXIA SIKEDA BIOTECH CO LTD
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