Synthesis
In a 1000 mL three-necked flask equipped with a thermometer, a mechanical stirrer, a reflux condenser tube and an off-gas absorption device, 540.56 g of m-methylbenzoic acid, 573.0 g of thionyl chloride and 1.0 g of N,N-dimethylformamide were added sequentially. The reaction mixture was heated to 90°C and the reaction was continuously stirred at this temperature for 3 hours. Upon completion of the reaction, the system was clear. The excess thionyl chloride was removed by distillation under reduced pressure, and 610.0 g of m-toluoyl chloride was finally obtained, which was determined to have a purity of 98.2% and a yield of 99.3%.
References
[1] Patent: CN107417518, 2017, A. Location in patent: Paragraph 0028
[2] Patent: CN105348085, 2016, A. Location in patent: Paragraph 0026; 0027; 0028; 0029; 0030
[3] Patent: CN107400052, 2017, A. Location in patent: Paragraph 0016
[4] Canadian Journal of Chemistry, 1963, vol. 41, p. 2962 - 2968
[5] Chemische Berichte, 1879, vol. 12, p. 2300
