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Processing method of 13C urea

A processing method and urea technology, applied in the directions of organic chemistry methods, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as expensive, biuret generation, and high cost of synthesis towers, and achieve high abundance and prevent decomposition. effect of reaction

Inactive Publication Date: 2017-05-10
JIANGSU HUAGEN TAILAI BIOTECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 13 The C urea breath test is used to check the infection of Helicobacter pylori, and its principle is to pass through the stable nuclide 13 The C-labeled substrate is introduced into the body (the main way is oral administration), and the final metabolite of the substrate is detected by an isotope ratio mass spectrometer 13 CO 2 Changes in the body to study metabolic reactions and physiological processes, the existing 13 C The urea production process is usually carried out under high temperature and high pressure conditions, and the reaction is carried out in a dedicated synthesis tower. The synthesis tower is expensive and uses expensive catalysts, and biuret impurities will be generated during the reaction process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Production 13 The method of C urea, comprises the following steps:

[0025] synthesis:

[0026] S1. Add 100 parts of sulfur in the reactor;

[0027] S2. Turn on the vacuum pump to evacuate the reactor, and the vacuum degree is 0.8-0.97;

[0028] S3. Add 900 parts of ethanol in the reactor;

[0029] S4. feed 7 parts of hydrogen sulfide gas, 15 parts of nitrogen and 180 parts of ammonia into the reactor;

[0030] S5. Add to the reactor 13 40 parts of CO gas, while heating the reactor, raise the temperature to 70°C, react for 1 hour, and the reaction ends;

[0031] S6. Stop heating the reactor and cool to 20°C;

[0032] Distillation:

[0033] S7. Send the reactant obtained in step S6 to a still, heat to 40° C., and carry out distillation under reduced pressure to obtain a solid mixture;

[0034] refined:

[0035] S8. Put the solid mixture obtained in step S7 into a reaction kettle, add distilled water and activated carbon, heat the temperature to 58° C., stir and ...

Embodiment 2

[0042] Production 13 The method of C urea, comprises the following steps:

[0043] synthesis:

[0044] S1. Add 100-120 parts of sulfur into the reactor;

[0045] S2. Turn on the vacuum pump to evacuate the reactor, and the vacuum degree is 0.8-0.97;

[0046] S3. Add 300 parts of methanol and 700 parts of ethanol in the reactor;

[0047] S4. Feed 7-12 parts of hydrogen sulfide gas and 180-240 parts of ammonia into the reactor;

[0048] S5. Add to the reactor 13 40-60 parts of CO gas, heat the reactor at the same time, raise the temperature to 70-90°C, react for 0.5-2 hours, and the reaction ends;

[0049] S6. Stop heating the reactor and cool to 20-40°C;

[0050] Distillation:

[0051] S7. Sending the reactant obtained in step S6 to a still, heating to 50-70° C., and performing vacuum distillation to obtain a solid mixture;

[0052] refined:

[0053] S8. Put the solid mixture obtained in step S7 into a reaction kettle, add purified water and activated carbon, heat the ...

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PUM

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Abstract

The invention discloses a processing method of 13C urea. The processing method comprises the following steps: under conditions of moderate pressure and moderate temperature, carrying out five paths of procedures including synthesis, distillation, refining, crystallization and drying on production raw materials including sulfur, alcohols, hydrogen sulfide, nitrogen gas, ammonia gas and 13CO to obtain the 13C urea. The production of the13C urea produced by the processing method does not need a special synthesis tower; reaction only needs to be carried out in a common reaction kettle and an expensive catalyst is not added; a carbamoylurea impurity is often generated in a common urea reaction process,but the processing method does not generate related impurities.

Description

technical field [0001] The invention relates to the field of pharmaceutical production, in particular to a production method under medium temperature and medium pressure conditions. 13 C urea method. Background technique [0002] 13 The C urea breath test is used to check the infection of Helicobacter pylori, and its principle is to pass through the stable nuclide 13 The C-labeled substrate is introduced into the body (the main way is oral administration), and the final metabolite of the substrate is detected by an isotope ratio mass spectrometer 13 CO 2 Changes in the body to study metabolic reactions and physiological processes, the existing 13 C The urea production process is usually carried out under high temperature and high pressure conditions, and the reaction is carried out in a dedicated synthesis tower. The synthesis tower is expensive and uses expensive catalysts. Biuret impurities will be generated during the reaction process. Contents of the invention [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C273/02C07C273/16
CPCC07C273/02C07B2200/05C07C273/16
Inventor 龚爱华马胜利
Owner JIANGSU HUAGEN TAILAI BIOTECH
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