BRUZINSKI, Paul,LIU, Xuejun,GIBB, Cameron,HERNANDEZ-ABAD, Pedro
申请号：
ES08719985
公开号：
ES2641190T3
申请日:
2008.03.13
申请国别(地区):
ES
年份:
2017
代理人:
摘要：
A chemical synthesis procedure of IB-MECA, which has the following formula (I): ** Formula ** comprising the procedure: (i) reacting 6-halopurine-9-riboside of the following formula (II): ** Formula ** in which X is a halogen selected from the group consisting of Cl, I and Br； with a diol protecting reagent to obtain a diol protected 6-halopurine of the following formula (III): ** Formula ** in which said diol protecting reagent comprises a linear or branched C1-C6 alkyl group； (ii) oxidizing the primary alcohol in said diol-protected 6-halopurine of formula (III) by adding a catalytic amount of an oxidizing agent consisting of sodium periodate and ruthenium trichloride (RuCl3) to obtain a respective derivative of carboxylic acid of formula (IV): ** Formula ** isolate said derivative by crystallization from water-acetonitrile； (iii) reacting the carboxylic acid group of the derivative of formula (IV), with a halogenating agent SOCl2 in acetonitrile to obtain an acid chloride followed by reaction with methylamine in the presence of diisopropylethylamine (DIPEA) to obtain the respective methylamide derivative of 6-halopurine protected with diol (III), the methylamide derivative having the formula (V): ** Formula ** replace the halogen group of the methylamide derivative (V) with 3-iodobenzylamine having <；= 0.5% of 3-bromobenzylamine hydrochloride, in the presence of DIPEA, the reaction mixture is heated to 70 ° C. (iv) forming a diol protected IB-MECA having the formula (VI)； ** Formula ** and allowing the diol protected IB-MECA of formula (VI) to recrystallize from MeOH； (v) removing the diol protection in the presence of aqueous hydrochloric acid to obtain said IB-MECA of formula (I) at a purity level of 99.67% and a yield of 90%.Un procedimiento de síntesis química de IB-MECA, que tiene la siguiente fórmula (I):**Fórmula** comprendiendo el procedimiento: (i) hacer reaccionar 6-halopurina-9-ribósido de la siguiente fórmula (II):**Fórmula** en la que X es un halóg
