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Development of an Optimized Process for 2,4-Dichloro-5-fluoroacetophenone: A Key Intermediate of Ciprofloxacin
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2024-07-24 , DOI: 10.1021/acs.oprd.4c00208 Kai Yin 1, 2, 3 , Youlan He 2 , Hao Wu 2 , Xubin He 3, 4 , Yiwei Zhang 1
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2024-07-24 , DOI: 10.1021/acs.oprd.4c00208 Kai Yin 1, 2, 3 , Youlan He 2 , Hao Wu 2 , Xubin He 3, 4 , Yiwei Zhang 1
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Herein, we report an optimized process for 2,4-dichloro-5-fluoroacetophenone, a key intermediate of ciprofloxacin. In the nitration step, the traditional mixed acid process was replaced by a microchannel continuous reaction technology. For the fluorination reactions, the traditional quaternary ammonium salt catalyst was replaced by a novel CNC+ catalyst, which led to improved catalytic efficiency, lowered reaction temperatures, and increased product yields. Furthermore, a cost-effective method for utilizing waste gases with high concentrations of nitrogen oxides was developed for the nitrochlorination reaction. In the acetylation step, magnetic materials featuring both Bronsted and Lewis acid sites were utilized to immobilize the bisacid site catalyst [HPhIm][FeCl4]/MPNs, replacing the traditional AlCl3 approach. The overall yield of this new sustainable process across all four steps reached 86.4%, marking a significant improvement of over 10% compared to the traditional method. Moreover, the new process has resulted in an 87% reduction in waste acid emissions and a remarkable 96% reduction in exhaust emissions.
中文翻译：
环丙沙星关键中间体 2,4-二氯-5-氟苯乙酮的优化工艺开发
在此，我们报告了环丙沙星关键中间体 2,4-二氯-5-氟苯乙酮的优化工艺。在硝化步骤中，采用微通道连续反应技术取代了传统的混酸工艺。在氟化反应中，新型CNC +催化剂取代了传统的季铵盐催化剂，提高了催化效率，降低了反应温度，提高了产品收率。此外，还开发了一种利用高浓度氮氧化物废气进行硝氯化反应的经济有效的方法。在乙酰化步骤中，利用具有布朗斯台德酸位和路易斯酸位的磁性材料来固定双酸位催化剂[HPhIm][FeCl 4 ]/MPNs，取代了传统的AlCl 3方法。这种新的可持续工艺的四个步骤的总体收率达到了 86.4%，与传统方法相比显着提高了 10% 以上。此外，新工艺还使废酸排放量减少了87%，废气排放量显着减少了96%。
更新日期：2024-07-24
中文翻译：
环丙沙星关键中间体 2,4-二氯-5-氟苯乙酮的优化工艺开发
在此，我们报告了环丙沙星关键中间体 2,4-二氯-5-氟苯乙酮的优化工艺。在硝化步骤中，采用微通道连续反应技术取代了传统的混酸工艺。在氟化反应中，新型CNC +催化剂取代了传统的季铵盐催化剂，提高了催化效率，降低了反应温度，提高了产品收率。此外，还开发了一种利用高浓度氮氧化物废气进行硝氯化反应的经济有效的方法。在乙酰化步骤中，利用具有布朗斯台德酸位和路易斯酸位的磁性材料来固定双酸位催化剂[HPhIm][FeCl 4 ]/MPNs，取代了传统的AlCl 3方法。这种新的可持续工艺的四个步骤的总体收率达到了 86.4%，与传统方法相比显着提高了 10% 以上。此外，新工艺还使废酸排放量减少了87%，废气排放量显着减少了96%。
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