Pentoxifylline as well as synthesis method and application thereof

A technology of pentoxifylline and a synthesis method, which is applied in the field of medicine, can solve the problems of dosage limitation, great personal harm and the like, and achieves the effects of simple synthesis process, few synthesis steps and low price

Pending Publication Date: 2022-04-22
赤峰万泽药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, pentoxifylline is usually synthesized by reacting with theobromine by preparing mesylate intermediates, but mesyla

Method used

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  • Pentoxifylline as well as synthesis method and application thereof
  • Pentoxifylline as well as synthesis method and application thereof
  • Pentoxifylline as well as synthesis method and application thereof

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preparation example Construction

[0038] The invention discloses a synthetic method of pentoxifylline, comprising the following steps:

[0039] Step 1: Synthesis of Intermediate Ⅰ

[0040] Add 6.5-7.5 parts of absolute ethanol, 2-3 parts of anhydrous potassium carbonate and 1-2 parts of ethyl acetoacetate into the reaction vessel, use absolute ethanol and anhydrous sodium carbonate, avoid the introduction of water, stir evenly, Then add 0.5-1.5 parts of 1,3-bromochloropropane, heat up to reflux reaction, the temperature is 70-80°C, the time is 7-8 hours, and the reaction product is separated and purified to obtain intermediate I;

[0041] Concrete reaction process is as follows:

[0042]

[0043] The specific steps of separation and purification are:

[0044] Cool the reaction product to room temperature (20°C ~ 30°C), collect the filtrate after centrifugation, in order to collect more fully, add absolute ethanol to the filter cake after the first centrifugation, stir and beat, reflux for 20 ~ 40min, and ...

Embodiment 1

[0069] Step 1: Synthesis of Intermediate Ⅰ

[0070] (1) Feeding 1: Turn on the vacuum pump, add 6.5 parts of absolute ethanol to the 1500L glass-lined reactor; open the solid feeding port and add 2 parts of anhydrous potassium carbonate (crushed through a 100-mesh sieve), and stir;

[0071] (2) Feeding 2: Add 1 part of ethyl acetoacetate at 20°C, after the addition is complete, stir at the temperature for 1 hour;

[0072] (3) Reaction: add 0.5 parts of 1,3-bromochloropropane, after the addition is complete, steam through the jacket, heat up to 70°C, and reflux for 7 hours;

[0073] (4) Separation and washing: Cooling water is passed through the jacket, the temperature is lowered to 20°C, centrifuged, the filter cake is stirred and beaten with 4 parts of absolute ethanol and refluxed for 30 minutes, and centrifuged;

[0074] (5) Concentration 1: Combine and collect the filtrate into a 5000L glass-lined glass-lined reaction kettle, pass steam, and concentrate under reduced pres...

Embodiment 2

[0105] Step 1: Synthesis of Intermediate Ⅰ

[0106] (1) Feeding 1: Turn on the vacuum pump, add 7.5 parts of absolute ethanol to the 1500L glass-lined reactor; open the solid feeding port and add 3 parts of anhydrous potassium carbonate (crushed through a 100-mesh sieve), and stir;

[0107] (2) Feeding 2: Add 2 parts of ethyl acetoacetate at 30°C, after the addition is complete, stir at the temperature for 2 hours;

[0108] (3) Reaction: Add 1.5 parts of 1,3-bromochloropropane, after the addition is complete, steam through the jacket, heat up to 80°C, and reflux for 8 hours;

[0109] (4) Separation and washing: Cooling water is passed through the jacket, the temperature is lowered to 30°C, centrifuged, the filter cake is stirred and beaten with 4.5 parts of absolute ethanol and refluxed for 40 minutes, and centrifuged;

[0110] (5) Concentration 1: Combine and collect the filtrate into a 5000L glass-lined glass-lined reaction kettle, pass steam, and concentrate under reduced ...

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Abstract

The invention discloses a synthesis method of pentoxifylline, which comprises the following steps: 1, synthesizing an intermediate I: adding 0.5-1.5 parts of 1, 3-bromochloropropane into 6.5-7.5 parts of absolute ethyl alcohol, 2-3 parts of anhydrous potassium carbonate and 1-2 parts of ethyl acetoacetate to carry out heating reflux reaction, and separating and purifying the reaction product to obtain the intermediate I; step 2, synthesizing an intermediate II: adding 0.5-1.5 parts of the intermediate I, 0.5-1.0 part of sodium bromide and 1-2 parts of 40-60% hydrobromic acid into the reaction container, dropwise adding concentrated sulfuric acid under a low-temperature condition until heat release is violent, carrying out heating reflux reaction, and separating and purifying a reaction product to obtain the intermediate II; and step 3, synthesizing pentoxifylline, namely dissolving 0.5-1.5 parts of theobromine in 2-3 parts of 10-30% sodium hydroxide solution, dropwise adding a mixed solution of 0.5-1.5 parts of the intermediate II and 4-5 parts of methanol, carrying out heating reflux reaction, and separating and purifying a reaction product to obtain the pentoxifylline. The synthesis process disclosed by the invention is relatively low in environmental pollution, and the synthesized pentoxifylline is relatively high in purity.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a pentoxifylline and its synthesis method and application. Background technique [0002] Pentoxifylline is an alkaloid synthesized by introducing pentanone groups into theobromine extracted from cocoa or tea leaves, which can improve blood circulation in the brain and limbs, increase blood flow in arteries and capillaries, and reduce peripheral vascular resistance; At the same time, it can also improve the deformability of pathologically damaged red blood cells, inhibit platelet aggregation, reduce blood viscosity, and increase the nutritional microcirculation in ischemic areas. Great clinical value. [0003] In the prior art, pentoxifylline is usually synthesized by reacting with theobromine by preparing mesylate intermediates, but mesylate is a carcinogen, and its dosage should be strictly limited during synthesis, and The synthesis process is more harmful to the...

Claims

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Application Information

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IPC IPC(8): C07D473/04A61K31/522A61P31/18A61P1/16
CPCC07D473/04A61P31/18A61P1/16
Inventor 张海立张赞波郭振军
Owner 赤峰万泽药业股份有限公司
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