10-羟基喜树碱的合成及光谱表征

喜树碱在30％过氧化氢氧化作用下生成喜树碱氮氧化物(OPT), 然后在浓硫酸催化下，光化学重排反应得到10-羟基喜树碱。通过正交实验，确定氧化反应最佳条件为：反应时间4 h，反应温度75 ℃，30％双氧水用量48 mL，溶剂乙酸用量350 mL(相对于0.01 mol喜树碱);光化反应条件：溶剂为V(1, 4-二氧六环)∶V(乙腈)∶V(H₂O)=6∶2∶1，浓硫酸为催化剂，经过硅胶柱层析提纯，回收率为49.9％，纯度为99.5％，熔点272～273 ℃。通过红外光谱、质谱, 一维、二维核磁共振波谱等手段对目标化合物的分子结构进行了表征，对化合物的红外光谱吸收峰及核磁谱线进行了归属分析，开发新的喜树碱衍生物提供了光谱依据。

Synthesis and Spectral Characterization of 10-Hydroxycamptothecin

10-hydroxycamptothecin was synthesized from camptothecin through oxidation and photo-activation. Grouping and optimizing the reaction conditions were as follows: in the oxidation condition: the reaction time 4 h, the reaction temperature 75 degrees C, the amount of H2O2 48 mL(w(H2O2) = 30%), the amount of HAc 350 mL(based on 0.01 mol CPT); in the photochemical reaction: the solvents V(1,4-dioxane): V(acetonitrile): V(H2O) = 6:2:1, bronsted acid catalyst 98% H2SO4. Purified by silica gel column, the total yield of HCPT is 49.9%, with 99.5% purity, m.p. 272-273 degrees C. The molecular structure of the title compound has been characterized by elemental analysis (EA), mass spectroscopy (MS), infrared spectrscopy(IR), and ID and 2D nuclear magnetic resonance spectrometry (NMR), and the main infrared absorption peaks and nuclear magnetic spectral bands of this conpound were assigned. The mass spectral fragmentations of the product's important fragment ions were elucidated. The result provides useful information for preparing the new derivatives of camptothecin.