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以邻溴苯胺为起始原料,经缩合、水解、N,N-二甲基-3-硝基-4-氯苯磺酰胺缩合、锌粉还原、铜催化Ullmann反应,得到目标化合物。并考察了缩合反应不同溶剂、碱、反应温度,还原反应还原剂的用量,Ullmann反应催化剂的用量、反应时间、反应温度对反应收率的影响。优化后5步反应总收率可达45.5%,且反应条件温和,后处理简便,在该工艺的中试生产中4批样品的车间总收率分别为38.2%、36.7%、36.9%、38.5%,且产品质量可靠,稳定性良好,产品经ESI-MS和1HNMR确证结构。
O-bromoaniline as the starting material, the condensation, hydrolysis, N, N-dimethyl-3-nitro-4-chlorobenzenesulfonamide condensation, zinc reduction, copper catalyzed Ullmann reaction, the target compound. The effects of different solvents, base, reaction temperature, the amount of reductant reductant, Ullmann reaction catalyst dosage, reaction time and reaction temperature on the yield of the reaction were investigated. After the optimization, the total yield of the five-step reaction can reach 45.5%, and the reaction conditions are mild and the post-treatment is simple. The total plant recovery of four batches of samples during the pilot production of the process are respectively 38.2%, 36.7%, 36.9% and 38.5 %, And the product quality is reliable, good stability, the product confirmed by ESI-MS and 1HNMR structure.