Crystal of dibutyryl adenosine cyclophosphate calcium salt

A dibutyryl cyclic adenosine phosphate calcium salt and crystal technology, which is applied in the field of crystalline powder of dibutyryl cyclic adenosine phosphate calcium salt, can solve problems such as unsuitable for large-scale production, hygroscopicity, instability, etc.

Active Publication Date: 2018-12-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these several methods can improve the HPLC purity to more than 90%, there are several problems, either the cost is high, and it is not suitable for large-scale production; The particle size is too poor, the bulk density is small, and the stability is poor; in most cases, the above three problems exist at the same time
[0005] Due to technical limitations, the current domestic standard for dibutyryl cyclic adenosine monophosphate calcium salt is still "Chemical Drug Landmark Upgrade National Standard Volume 9", the version is relatively old, and the standard for product specifications is relatively low - "calculated as dry product, containing C18H23N5O8P 1/2Ca must not be less than 80.0%, light yellow powder, with spec...

Method used

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  • Crystal of dibutyryl adenosine cyclophosphate calcium salt
  • Crystal of dibutyryl adenosine cyclophosphate calcium salt
  • Crystal of dibutyryl adenosine cyclophosphate calcium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Take 150g of crude dibutyrylcyclic adenosine monophosphate calcium salt, add it to 1000mL of absolute ethanol, and fully dissolve it at 50°C. The process is carried out in a 1.5L crystallizer with a jacket, and the stirring speed is controlled at 200r / min. A three-curved impeller impeller is used with a diameter of 80 mm. The top of the crystallizer is equipped with a condensation reflux device, and the temperature of the jacket of the crystallization system is controlled by cooling circulating water. After dissolving for 10 minutes, slowly lower the temperature at a rate of 2°C / h, and at the same time pump in isopropanol at a flow rate of 2.0mL / min. The volume of added isopropanol is 800-1200mL. Then put it into the tank, carry out solid-liquid separation by suction filtration, wash the filter cake with 400mL of anhydrous acetone, then place it in a blast drying oven at 35°C, and dry it for 4h with an airflow with a relative equilibrium humidity RH of 65%, and then obta...

Embodiment 2

[0065] Take 300g of crude dibutyrylcyclic adenosine monophosphate calcium salt, add it to 1000mL of water, and fully dissolve it at 10°C. The process is carried out in a 2L crystallizer with a jacket, and the stirring speed is controlled at 200r / min, using a two-leaf anchor Stirring paddle, paddle diameter is 90mm, crystallization system jacket adopts cooling circulating water to control temperature. After fully dissolving for 30 minutes, slowly raise the temperature at a rate of 2°C / h until the temperature rises to 60°C, maintain for 2 hours, then put it into the tank, and separate the solid and liquid by suction filtration, using 300mL methanol aqueous solution with a methanol volume fraction of 95%. Wash the filter cake, then place it in a blast drying oven at 40°C, and dry it with an airflow with a relative equilibrium humidity RH of 45% for 4 hours, and then obtain the pure product of dibutyrylcyclic adenosine phosphate calcium salt, and determine the moisture content by K...

Embodiment 3

[0067] Take 100g of the crude product of dibutyrylcyclic adenosine monophosphate calcium salt, add it into 1000mL n-propanol ethanol solution (the mass ratio of n-propanol and ethanol is 1:1), fully dissolve at 50°C, the process is in a jacketed 1.5 It is carried out in a crystallizer of L, the stirring speed control is set at 250r / min, and the temperature of the jacket of the crystallization system is controlled by cooling circulating water. After fully dissolving for 15 minutes, first cool down to 35°C at a rate of 2°C / h, then cool down to 10°C at a rate of 1°C / h, keep for 2 hours, and then put it into the tank, and separate the solid and liquid by suction filtration. Wash the filter cake with 250mL of absolute ethanol, then place it in a blast drying oven at 50°C, and dry it with an airflow with a relative equilibrium humidity RH of 55% for 4 hours, and then obtain the pure product of dibutyrylcyclic adenosine monophosphate calcium salt, Karl Fei The moisture content determ...

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Abstract

The invention relates to a crystal of a dibutyryl adenosine cyclophosphate calcium salt, the structural formula of the crystal is C72H92Ca2N20O32P4.9H2O, belongs to an orthorhombic crystal system anda P212121 space group, the cell parameters are shown in the description, alpha=beta=gamma=90 degrees, Z=4, the cell volume V is shown in the description , R=0.07, the true density of the crystal is 1.455 kg/m<3>, each cell comprises four minimal asymmetric units, and each minimal asymmetric unit further comprises 4 dibutyacyl adenosine cyclphosphate anions, 2 calcium ions, and 9 crystal water. Thestacking density of the crystal powder is more than 0.35 g/mL, the tap density is more than 0.38 g/mL, and the HPLC purity is more than 99.2%.

Description

technical field [0001] The invention belongs to the refining field of medicine and feed additives, and specifically relates to a crystal structure of dibutyryl cyclic adenosine phosphate calcium salt, a crystalline powder of dibutyryl cyclic adenosine phosphate calcium salt, and a preparation method thereof. Background technique [0002] Calcium Dibutyacyladenosine Cyclophosphate (DbcAMPCa), scientific name N 6 , 2′-O-Dibutyryladenosine-3′, 5′-cyclic monophosphoric acid, calcium, the molecular structure formula of its monovalent anion is attached figure 1 , is a derivative of cyclic adenosine monophosphate (cAMP), because it has better cell membrane permeability than cyclic adenosine monophosphate, and can resist the hydrolysis of phosphodiesterase in vivo, so its action time and speed are longer than cAMP And quickly, because it has significant effects in the treatment of heart disease, immune diseases, etc. (CN101172112A). [0003] The current preparation methods basical...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
CPCC07B2200/13C07F9/65744
Inventor 杨朋朋应汉杰林晨光沈涛李晓洁李子涵朱晨杰柳东欧阳平凯
Owner NANJING UNIV OF TECH
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