Process of preparing dibutyryl adenosine cyclophosphate

Abstract

The invention relates to a preparation method of dibutyryl cyclic adenosine monophosphate using cyclic adenosine monophosphate as raw material. The technical problem solved by the invention is to reduce the consumption of anhydrous pyridine with bad smell and improve the yield of the product. The method of the present invention is, 1) salt forming; 2) acylation reaction: a route—according to the weight of cyclic adenosine monophosphate triethylamine salt: the volume of butyric anhydride: the ratio of pyridine volume=1: 8~20: 3~7 feeding intake , react fully to obtain an acylation reaction solution; or route B—freeze-dry the triethylamine salt of adenosine cyclic monophosphate, and add it according to the ratio of triethylamine salt of cyclic adenosine monophosphate: volume of butyric anhydride = 1:8-20 Butyric anhydride, fully reacted to obtain an acylation reaction solution; 3) Extraction: adding one or more mixtures of ethers, hydrocarbons, and esters containing five or more carbon atoms for extraction, adding kerosene, and washing for many times Dibutyryl cyclic adenosine monophosphate.

Description

technical field [0001] The invention relates to a pharmaceutical preparation, in particular to a preparation method of dibutyryl cyclic adenosine monophosphate (DB-cAMP) using cyclic adenosine monophosphate as a raw material. Background technique [0002] A kind of preparation method of dibutyryl cyclic adenosine monophosphate is disclosed in CN1554358 " cyclic adenosine monophosphate calcium preparation and preparation method ", (1) preparation of quaternary ammonium salt: cyclic adenosine monophosphate is added triethylamine to make it dissolve, and then Add anhydrous pyridine, remove pyridine under reduced pressure at 30-70°C, and dry to obtain cyclic adenosine monophosphate triethylamine salt; (2) Acylation-hydrolysis: take cAMP triethylamine salt, add anhydrous pyridine and butyric anhydride, avoid Light reaction for 4 to 10 days, after complete acylation reaction, take out the reaction solution, add distilled water, hydrolyze for 2 to 3 hours, then concentrate under re...

AI Technical Summary

Problems solved by technology

[0004] Product yield is not high enough (only about 67%) in the above-mentioned technology, and the smell of anhydrous pyridine is unpleasant, is restricted in use

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