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使用壁厚为1~1.5μm,断面内径为0.5~1.5 mm的玻璃毛细管,制作了简易微管连续流反应器。利用该连续流反应器合成了13个查耳酮,并应用IR和1HNMR谱对所合成的化合物进行了结构表征。结果表明,在40kHz的超声波作用下,反应温度26~38℃,使用该反应器合成查耳酮的产率可高达80%~90%,与传统的烧瓶反应相比,反应时间由原来的1~6 h缩短到10 min左右。该法反应产率高、反应时间短,可以连续、大规模合成查耳酮。
A simple microtube continuous flow reactor was fabricated using glass capillaries with a wall thickness of 1 to 1.5 μm and a cross section of 0.5 to 1.5 mm. Thirteen chalcone ketones were synthesized by the continuous flow reactor. The synthesized compounds were characterized by IR and 1HNMR. The results show that the reaction temperature is 26 ~ 38 ℃ under ultrasonic wave of 40kHz, and the yield of chalcone can be as high as 80% ~ 90%. Compared with the traditional flask reaction, the reaction time is from 1 ~ 6 h shortened to 10 min or so. The method of high yield, short reaction time, continuous, large-scale synthesis of chalcone.