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A kind of preparation method of theophylline sodium salt

A technology of sodium theophylline and sodium nitrite, applied in the field of medicine and chemical industry, can solve the problems of low product yield, high content of by-products, strong smell of product ammonia and the like

Active Publication Date: 2021-05-04
河北广祥制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems that the reaction process is difficult to control, the product yield is low, the content of by-products is high, the product has a strong ammonia smell and a large amount of waste gas pollutants exists in the existing synthetic method of theophylline sodium salt, the present invention provides a kind of theophylline sodium salt Preparation

Method used

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  • A kind of preparation method of theophylline sodium salt
  • A kind of preparation method of theophylline sodium salt
  • A kind of preparation method of theophylline sodium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Add 1500g of 70wt% cyanoacetic acid into a 20L glass reactor, the temperature is 70°C, the vacuum degree is 0.095MPa, when the water is distilled under reduced pressure until no fraction is extracted, add 800mL of acetic acid to continue the distillation under reduced pressure, and use acetic acid to take out the residual Moisture, temperature 90°C, vacuum degree 0.095MPa, distill until no distillate is extracted. The temperature was lowered to 40°C, 1365 g of acetic anhydride was added to the dehydrated cyanoacetic acid, and the reaction was stirred for 20 minutes. Turn on the vacuum, distill the acetic acid generated by the reaction under reduced pressure, control the temperature between 70-90°C, and the vacuum degree between 0.095-0.2MPa until no distillate is extracted. 1050 g of 1,3-dimethylurea was added, the temperature was controlled at 40°C, and the reaction was stirred for 30 minutes. The acetic acid generated by the reaction is distilled off under reduced pr...

Embodiment 2

[0052] Add 1500g of 70wt% cyanoacetic acid to a 20L glass reactor, the temperature is 50°C, and the vacuum degree is 0.1MPa. Moisture, the temperature is 80°C, the vacuum is 0.1MPa, distill until no distillate is recovered. At 100°C, 1575 g of acetic anhydride was added to the dehydrated cyanoacetic acid, and the reaction was stirred for 60 minutes. Turn on the vacuum, distill the acetic acid generated by the reaction under reduced pressure, control the temperature between 70-90°C, and the vacuum degree between 0.095-0.2MPa until no distillate is extracted. 1260 g of 1,3-dimethylurea was added, the temperature was controlled at 100°C, and the reaction was stirred for 120 min. The acetic acid generated by the reaction is distilled off under reduced pressure, the temperature is controlled between 70-90°C, and the vacuum degree is between 0.095-0.2MPa until no distillate is extracted.

[0053] Add 300mL of water to the reaction liquid, carry the acid with the water, control the...

Embodiment 3

[0059] Add 1500g of 70wt% cyanoacetic acid into a 20L glass reactor, the temperature is 60°C, the vacuum degree is 0.15MPa, when the water is distilled under reduced pressure until no fraction is extracted, add 800mL of acetic acid to continue the distillation under reduced pressure, and use acetic acid to take out the residual Moisture, the temperature is 90°C, the vacuum is 0.1MPa, distill until no distillate is recovered. Cool down to 70°C, add 1500 g of acetic anhydride to the dehydrated cyanoacetic acid, and stir for 35 minutes. Turn on the vacuum, distill the acetic acid generated by the reaction under reduced pressure, control the temperature between 70-90°C, and the vacuum degree between 0.095-0.2MPa until no distillate is extracted. 1150 g of 1,3-dimethylurea was added, the temperature was controlled at 70°C, and the reaction was stirred for 70 min. The acetic acid generated by the reaction is distilled off under reduced pressure, the temperature is controlled betwee...

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Abstract

The invention relates to the technical field of medicine and chemical industry, and specifically discloses a preparation method of theophylline sodium salt. The preparation method of theophylline sodium salt comprises the following process steps: mixed reaction of cyanoacetic acid and acetic anhydride to obtain mixed acid anhydride, condensation reaction of mixed acid anhydride and 1,3-dimethylurea to obtain 1,3-dimethylcyanoacetyl Urea; 1,3-dimethylcyanoacetylurea obtains 1,3-dimethyl-4-amino-5-carboxamidoureazine by cyclization, nitrosation reaction, hydrogenation and acylation successively, and described 1,3-dimethyl-4-amino-5-carboxamidoureazine ring-closed to obtain theophylline sodium salt. The preparation method of theophylline sodium salt of the present invention has the advantages of mild reaction conditions, easy control, high product yield, less by-products, no strong ammonia smell, low cost and less polluting waste.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a preparation method of theophylline sodium salt. Background technique [0002] Theophylline sodium salt is an important intermediate structure of xanthine drugs, which can be used to synthesize caffeine, theobromine, theophylline, doxofylline, aminophylline, 8-chlorophylline and other products. [0003] The existing synthetic method of theophylline sodium salt is to add acetic anhydride and 1,3 dimethylurea to carry out condensation reaction to obtain 1,3-dimethyl cyanoacetyl urea after dehydration of cyanoacetic acid aqueous solution; 1,3-dimethyl cyanoacetyl urea Cyclization under basic conditions gives 1,3-dimethyl-4-iminouracil, and 1,3-dimethyl-4-iminouracil undergoes nitrosation reaction with sodium nitrate under acidic conditions to obtain 1,3 -Dimethyl-4-imino-5-isonitrosourazine; 1,3-dimethyl-4-imino-5-isonitrosourazine after repeated beating and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04
CPCC07B2200/13C07D487/04
Inventor 韩淑芹韩悦朱树杰张维金付里航马献国
Owner 河北广祥制药有限公司