doi:10.16597/j.cnki.issn.1002-154x.2022.06.003
连续流动微反应器中安全高效合成对甲基苯甲酰氯和正辛酰氯
蔡嘉良1 王楠1 戎有明2 周建成1,2 李乃旭1,2∗
(1. 东南大学 化学化工学院,江苏 南京 211189; 2. 中微纳米功能材料研究院有限公司,江苏 南京 210044)
Safe and Efficient Synthesis of p-toluoyl Chloride and n-octanoyl Chloride in a Continuous Flow Microreactor
Cai Jialiang 1; Wang Nan 1; Rong Youming 2; Zhou Jiancheng 1,2; Li Naixu 1,2∗;
(1. School of Chemistry and Chemical Engineering, Southeast University, Jiangsu Nanjing 211189; 2. Nanjing Zhongwei Nano Functional Materials Research Institute Co. Ltd, Jiangsu Nanjing 210044)
摘要:
酰氯类化合物是非常重要的有机合成中间体,在医药、农药、化工材料等方面有着广泛应用。 在微反应体系 中使用固体光气(BTC)制备对甲基苯甲酰氯/ 正辛酰氯可以实现对反应的高度控制,大大提高反应的安全性。 我们采用了二甲基甲酰胺(DMF)和 BTC 的反应体系避免了反应器的堵塞,提高了反应过程的效率。 改变反应条件(不同的催化剂,DMF 用量,停留时间,反应温度,R-COOH 与 BTC 的摩尔比)以改进目标产物的合成产率,在最优条件下,对甲基苯甲酰氯产率可达到 87.36% ,正辛酰氯产率可达到 93.49% 。
关键词：对甲基苯甲酰氯 正辛酰氯 微反应器 固体光气
Abstract：
Acyl chloride is an important intermediate in organic synthesis, which has a wide range of applications in medicine, pesticides, and chemical materials. Using Triphosgene ( BTC ) to prepare p-toluoyl chloride / n-octanoyl chloride in a micro-reaction system can achieve a high degree of control over the reaction and significantly improve the safety. In this paper, we adopted the Dimethylformamide (DMF) / BTC reaction system to avoid the clogging of the reactor and to improve the efficiency. Different reaction conditions, such as the amount of DMF, the type of catalyst, the residence time, the reaction temperature, the M-ratio ( R-COOH / BTC), were investigated to improve the synthesis of the target product. Under the optimal conditions, the yield of p-toluoyl chloride reached 87. 36% , and the yield of n-octanoyl chloride achieved 93. 49% .
Keywords：p-toluoyl chloride; n-octanoyl chlorid; microreactor; BTC;