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Method for synthesizing diprophylline

A technology of diprophylline and theophylline, which is applied in the field of synthesis of pharmaceutical compounds to achieve the effects of shortening the reaction time, simplifying the subsequent refining process, and high product yield and purity

Active Publication Date: 2011-11-09
HUNAN ER KANG PHARMA
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Problems solved by technology

But the product yields obtained by these methods are all lower, all below 70%.

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  • Method for synthesizing diprophylline
  • Method for synthesizing diprophylline

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Embodiment

[0032] According to the following operating steps, the operating conditions listed in Table 2 were used to synthesize diprophylline.

[0033] Put 400ml of pure water into a 1000ml three-necked bottle equipped with a stirrer, a condenser and a dropping funnel, start stirring, add sodium hydroxide, add 181g (1mol) of theophylline after it is completely dissolved, and heat up to 110-120°C Insulation reaction 30min. Then control the temperature at 75-90°C, and slowly add monochloropropanediol. The reaction is then stirred for a period of time at the condensation temperature. After the stirring reaction is complete, control the vacuum degree above -0.085Mpa and distill until the material is white viscous. After distillation under reduced pressure to the end point, slowly add 550ml of ethanol, keep warm and reflux for 30 minutes to completely dissolve the product in the material, press filter, grow crystals, centrifuge, dry and pulverize to obtain the finished product.

[0034] T...

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Abstract

The invention relates to a method for preparing diprophylline, which comprises the step of: converting theophylline into a theophylline salt by strong alkali selected from sodium hydroxide and potassium hydroxide and the steps of condensing the theophylline salt and dichlorohydrin; the method is characterized in that the mole ratio of the theophylline, the strong alkali and the dichlorohydrin is 1:1.05 to 2.0:1.05 to 2.0; in addition, the temperature for converting and salinization is 80 to 130 DEG C and the temperature for condensation is 90 to 110 DEG C. The method can obtain relatively highproduct yield and purity, shorten condensation reaction time and simplify the subsequent fining technique of finished products.

Description

technical field [0001] The present invention relates to a kind of synthetic method of medicine compound, more specifically relate to a kind of synthetic method of theophylline derivative. Background technique [0002] Dihydroxypropyl theophylline, also known as glycerol theophylline, phenidine, chemical name 1,3-dimethyl-7-(2,3-dihydroxypropyl)-3,7-dihydro-1H-purine-2 , 6-diketone. Dihydroxyprophylline, a derivative of theophylline, is a smooth muscle relaxant that can promote the release of endogenous adrenaline substances. Its effect is basically similar to that of aminophylline, and its bronchodilation effect is weaker than that of aminophylline, which is only 10% to 20% of that of aminophylline. The adverse reaction is small, and its toxicity is 20% to 25% of that of aminophylline. It has less influence on the heart and nervous system, and is especially suitable for asthmatic patients with tachycardia. It is clinically used for bronchial asthma and cardiac asthma, et...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D473/08
Inventor 帅放文王向峰章家伟
Owner HUNAN ER KANG PHARMA
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