METHOD OF MANUFACTURING 9-(2-HYDROXY ETHOXY METHYL)GUANINE
PURPOSE: The highly pure 9-(2-hydroxy ethoxymethyl)guanine is produced by simplification of reaction process and converting the by-product of reaction into the wanted intermediate. CONSTITUTION: Guanine of 151.13g is refluxed in the mixed solutions of N,N-dimethyl form amide of 1000ml and acetic anh...
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| Zusammenfassung: | PURPOSE: The highly pure 9-(2-hydroxy ethoxymethyl)guanine is produced by simplification of reaction process and converting the by-product of reaction into the wanted intermediate. CONSTITUTION: Guanine of 151.13g is refluxed in the mixed solutions of N,N-dimethyl form amide of 1000ml and acetic anhydride of 360ml for 3 hours and cooled to 80°C. 2-Oxo-1,4-butanediol diacetate of 460g and p-toluene sulfonic acid of 2g are added into the reaction liquid and heated to 120°C to give N¬2-acetyl-9-(2-acetoxy ethoxy methyl)guanine of the formula (IV).
본 발명은 구아닌에 무수초산를 첨가하여 디아세틸 구아닌을 합성한후 2-옥사-1,4-부탄디올 디아세테이트와 반응시켜 N-아세틸-9-(2-아세톡시 에톡시 메틸) 구아닌을 생성하고 탈 아세틸화 과정을 거쳐 다음 9-(2-하이드록시 에톡시 메틸) 구아닌을 제조하는 방법으로서, 반응공정을 단순화하고 반응중 생성된 부산물을 분리 제거하지 않고 원하는 중간체로 99%이상 전환시킴으로써 고순도의 9-(2-하이드록시 에톡시 메틸) 구아닌을 고수율로 얻을수 있는 방법이다. |
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