苯菌酮的合成工艺

Synthesis of Metrafenone

以2-甲氧基-6-甲基苯甲酸和3,4,5-三甲氧基甲苯为原料,经过溴化反应、酰氯化反应和傅克反应制备得到标题化合物。通过对单元反应的条件优化,确认了最佳合成工艺:溴化反应中,以二氯乙烷为最佳反应溶剂,催化剂干燥铁粉最佳用量为14.3 mmol;酰氯化反应中,磺酰氯为最佳的氯化试剂;傅克反应中,最佳催化剂为四氯化钛,催化剂用量为2.2mmol。3步反应总收率为77.1%,化合物结构经过~1HNMR和^(13)CNMR确证。

2-Methoxy-6-methylbenzoic acid and 3,4,5-trimethoxytoluene were used as raw materials to prepare benzenone by bromination,acyl chlorination and Foucault reaction.The optimum reaction conditions were determined by optimizing the conditions of the unit reaction.In the bromination reaction,dichloroethane was used as the optimum reaction solvent,and the optimum amount of catalyst dry iron powdewas 14. 3 mmol.The optimum chlorination reagent sulfonyl chloridewas used in the acid chlorination reaction.Titanium tetrachloride was the best catalyst and the best catalyst dosage is 2. 2 mmol in the Foucault reaction.The total yield of the 3-step reaction was 77. 1%,and the structure of the compound was confirmed by ~1HNMR and ^（13）CNMR.