阿扎胞苷-技术总结(共2篇) .: .: .:Wt.: NH2NNN NaOMeNAcOHOMe 3 .:Wt.: 步骤1操作程序: Ina22L,3-neckedflask,amixtureof5-azacytosine(1)(kg,mol,molareq.),HMDS(kg)andammoniumsulfate(g)(g)wasadded,,pale-yellow,-whiteresidue,whichistrimethylsilylated5-azacytosine. 步骤2操作程序: Trimethylsilylated5-azacytosine(6)ordingtothemethodofExample1wasdilutedwithanhydrousdichloromethane(kg)ina50L,3-necked,flaskandsolid,1,2,3,5-Tetra-O-acetyl-β-D-ribofuranose(kg,mol)(7)(kg)wasusedandtheslurrywascooledto0-5℃.TMS-triflate(kg,molareq.)wasaddedtothemixtureover5-,thereactiontemperature increasedto15-20℃.andtheinitialsuspensionturnedintoaclear,pale-yellow,,thesolutionWaspouredoveramixtureofNa2C03(kg),NaHC03(kg),water(kg)andice(kg).(kg).anicswerewashedwithcold(0-5℃.)10%NaHC03(2xl0L).binedwashingswereextractedwithdichloromethane(kg).anicswerewashedwithcoldwater(2x5kg),driedonMgS04(kg),(kg)binedandreducedinvolumeusingvacuum(-200mmHg,30℃).Thedist
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