Calcium dibutyryladenosine cyclophosphate preparation method

A technology of calcium dibutyryl cyclic adenosine phosphate and calcium cyclic adenosine phosphate, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of cumbersome process, poor product quality, and consumption cost, and achieve High reaction selectivity, short reaction time, and cost-saving effects

Active Publication Date: 2017-01-18
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The traditional synthetic route is to make ethylamine salt first, then acylate and then make calcium salt. Not only is the process cumbersome and the yield is low, but a...

Method used

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  • Calcium dibutyryladenosine cyclophosphate preparation method
  • Calcium dibutyryladenosine cyclophosphate preparation method
  • Calcium dibutyryladenosine cyclophosphate preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Accurately weigh cyclic adenosine monophosphate and calcium hydroxide in a beaker, and add a certain amount of water to the beaker, wherein the molar ratio of cyclic adenosine monophosphate and calcium hydroxide is 1:1.2, the mass of cyclic adenosine monophosphate and water Ratio 1:6, vigorously stirred for about 30 minutes, filtered the reaction solution, and removed the filter residue.

Embodiment 2

[0038] To the above filtrate, add ethanol dropwise to crystallize and stir vigorously, the volume ratio of ethanol to filtrate is 3:1, filter the precipitated cyclic adenosine monophosphate calcium salt, and vacuum dry at 60-80°C to obtain the product cyclic adenosine monophosphate Calcium salt, the conversion rate is 100%, and the selectivity is >99%. The liquid phase diagram of calcium cyclic adenosine monophosphate is shown in image 3 .

Embodiment 3

[0040] The acylation reaction is carried out in a three-necked flask. One of the three-necked flasks is connected to a condenser, the other is protected by nitrogen gas, and the other is fed with materials. The reaction is heated in an oil bath and stirred by a magnetic stirrer.

[0041] The reaction device is as shown above, weigh a certain amount of cyclic adenosine monophosphate calcium in the flask, and add a certain volume of butyric anhydride to it, wherein the mass volume ratio of cyclic adenosine monophosphate calcium and butyric anhydride is 1g:10ml, react respectively React at 120° C., 130° C., and 140° C. for 3 hours. After the reaction, samples were taken for detection. The conversion and selectivity are shown in Table 1.

[0042] Selectivity and conversion rate of table 1 embodiment 3

[0043] temperature reflex Conversion rates selectivity 120℃ 63.2％ 87.4％ 130℃ 89.7％ 92.4％ 140℃ 97.6％ 94.6％

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Abstract

The invention discloses a calcium dibutyryladenosine cyclophosphate preparation method, which is characterized by comprising: (1) adding adenosine cyclophosphate and calcium hydroxide to water according to a molar ratio of 1:1-1.2, carrying out a reaction for 30-40 min, filtering to remove insoluble matters, adding ethanol having the volume 2-3 times the volume of the filtrate to the filtrate, filtering after a calcium adenosine cyclophosphate salt is precipitated, and carrying out vacuum drying at a temperature of 60-80 DEG C to obtain calcium adenosine cyclophosphate; (2) adding the calcium adenosine cyclophosphate obtained in the step (1) and butyric anhydride to a reaction kettle according to a ratio of 1 g:7-12 ml, protecting with nitrogen, and carrying out a stirring reaction for 1-3 h; and (3) adding 0-4 DEG C water having the volume 3-4 times the volume of the reaction liquid obtained in the step (2) to the reaction liquid, stirring for 30-40 min, carrying out nano-filtration on the reaction liquid, concentrating the trapping liquid, and carrying out freeze drying or spray drying to obtain the calcium dibutyryladenosine cyclophosphate. According to the present invention, the selectivity of the obtained calcium dibutyryladenosine cyclophosphate is more than 90%, the reaction time is short, the reaction process is simple and environmental friendly, and the method is suitable for industrial application.

Description

technical field [0001] The invention belongs to the field of biochemical industry, and specifically relates to a method for preparing cyclic adenosine phosphate calcium from cyclic adenosine monophosphate and performing acylation reaction with butyric anhydride to obtain dibutyryl cyclic adenosine phosphate calcium as a product. Background technique [0002] Cyclic Adenosine-3',5'-Mconophosphate (cAMP for short) is a derivative of nucleotides, which is an important substance in the human body that can transmit nitrogen-containing hormones. When the nitrogen-containing hormone is secreted from a certain cell, it travels to the target cell with the body fluid, and when it acts on the specific receptor on the cell membrane, it activates the adenylyl cyclase in the cell membrane. 2+ or Ca 2+ Under the condition of existence, the adenosine triphosphate (ATP) in the cell is converted into cAMP, and then protein kinase is activated by cAMP, and various enzyme systems are activated...

Claims

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Application Information

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IPC IPC(8): C07H1/00C07H19/213
CPCC07H1/00C07H19/213
Inventor 应汉杰朱晨杰沈涛杨朋朋周精卫牛欢青
Owner NANJING UNIV OF TECH
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