摘要
3-甲氧基-2-甲基-苯甲酰氯是合成甲氧虫酰肼的关键中间体。以2,6-二氯甲苯为原料,经醚化、格氏反应、水解和酰氯化反应合成了3-甲氧基-2-甲基-苯甲酰氯;通过单因素实验确定了各步反应的工艺条件。醚化反应以N,N-二甲基乙酰胺为溶剂,反应温度为130℃,反应时间为6.0 h,收率为97.1%;格氏交换、水解的原料配比n(6-氯-2-甲氧基甲苯)∶n(Mg)=1∶1.05,反应时间为3.0 h,通二氧化碳温度为-5~0℃,收率为93.2%;酰氯化反应的原料配比n(3-甲氧基-2-甲基苯甲酸)∶n(SOCl2)=1∶1.10,反应温度为50℃,收率为98.3%。经优化后,反应总收率为88.9%,纯度为99.2%。该工艺原料价廉易得,反应路线短,条件温和,收率高,成本低,环境友好,适合工业生产。
3-methoxy-2-methyl-benzoyl chloride is a key intermediate for synthesizing methoxyfenozide.3-methoxy-2-methyl-benzoyl chloride was synthesized with 2,6-dichlorotoluene as the material in the processes of etherification,Grignard reaction,hydrolysis,and acylating chlorination reaction successively,and the process conditions of each of the reaction stages were identified by single-factor experiment.N,N-dimethylacetamide was used as the solvent in etherification reaction,the reaction temperature was 130℃,the reaction time was 6.0 h,and the yield was 97.1%.The material ratio in Grignard reaction and hydrolysis was n(CMT):n(Mg)=1:1.05,the reaction time was 3.0 h,carbon dioxide ventilation temperature was-5~0℃,and the yield was 93.2%.The material ratio in acylating chlorination reaction was n(MMBC):n(SOCl2)=1:1.10,the reaction temperature was 50℃,and the yield was 98.3%.The overall yield was 88.9%and the purity was 99.2%after optimization.The materials for this technology are cheap and easy to acquire.The reaction route is short,the reaction conditions are moderate,the yield is high,the cost is low,and the technology is environment friendly and therefore is suitable for industrial production.
作者
杜友兴
何立
DU Youxing;HE Li(Shanghai Chemspec Corporation,Shanghai 200331)
出处
《精细石油化工进展》
CAS
2020年第2期46-49,57,共5页
Advances in Fine Petrochemicals
