【摘要】 介绍了一种以无机硝酸盐为硝化剂、喜树碱为原料、浓硫酸为溶剂合成9?硝基喜树碱(9?NC)的新方法.在此硝化反应体系中,合成9?NC的最佳工艺条件为喜树碱0.5g,浓硫酸40mL,?NO3?0.007mol,KNO3/Sr(NO3)2为1:1.在冰盐浴下反应4h,再于40℃下反应1d得到9?NC初产物,经柱层析后,产品收率为41.1%,9?NC纯度98.8%(ω),均高于文献值.更多还原

【Abstract】 A new method for synthesizing 20(S)-9-Nitro-camptothecin was proposed by using inorganic nitrates as nitration reagents, camptothecin as the raw material, and concentrated sulfuric acid as solvent. The best reaction conditions were: camptothecin 0.5 g, concentrated sulfuric acid 40 mL, ?NO3? 0.007 mol, and KNO3/Sr(NO3)2 1:1 (molar ratio). The nitration procedure was carried out in ice-salt bath for 4 h and then at 40℃ for 1 d. The crude nitration products were purified by column chromatography. The total yield of nitration products was 41.1% (40% in the literature) with 98.8% (98% in the literature) purity for 9-NC.更多还原