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以芦丁为原料,甲醇钠调pH=9.5,54℃与苯甲酰氯反应,薄层色谱(TLC)板监测反应完毕,过滤、乙醇/丙酮重结晶。紫外光谱(UV)显示芦丁的两个特征吸收峰均发生蓝移,这是形成新化合物共轭体系变化引起的。IR中νOH峰明显减弱,说明芦丁中多个羟基发生了反应,νc=o位于1 755.36cm~(-1),酯羰基峰明显增强;νc—o位于1 219.18cm~(-1),变宽增强。1 H NMR中7-OH、3′-OH、4′-OH上面的氢消失,说明与苯甲酰氯发生了酯化反应,同时,在7.6~8.8处有苯甲酰基的多重峰。MS中m/z:921.2为芦丁三苯甲酸酯的分子离子峰。
To rutin as raw material, sodium methylate pH = 9.5, 54 ℃ with benzoyl chloride reaction, TLC monitoring reaction was completed, filtered, ethanol / acetone recrystallization. UV spectroscopy (UV) showed that both peaks of rutin were blue-shifted, which was caused by the change of conjugate system of new compounds. The peak of νOH in IR was obviously weakened, which indicated that many hydroxyl groups in rutin reacted. Νc = o was located at 1 755.36cm -1 and the ester carbonyl peak was obviously enhanced. Νc-o was at 1 219.18 cm -1, Widening The hydrogen in the 7-OH, 3’-OH and 4’-OH in the 1 H NMR disappeared, indicating esterification with benzoyl chloride and a multiplet of benzoyl at 7.6-8.8. M / z in MS: 921.2 is the molecular ion peak of rutin tribenzoate.