The synthesis of the pharmaceutically relevant scaffold 3,4-dihydro-1H-1-benzazepine-2,5-dione via Krapcho dealkoxycarbonylation in a continuous high temperature high pressure coil reactor is investigated and compared to results from batch experiments. In a first step, the continuous reactors residence time distribution (RTD) is characterized, followed by an initial comparison of batch and continuous reactant conversion profiles indicating a very good agreement between both reactors by means of conversion time. Reaction temperature is increased above the solvents atmospheric boiling point in the continuous reactor system to intensify the reaction and increase throughput. Optimal reaction parameters for complete conversion of the starting material in ≤ 3 min reaction time were estimated based on batch kinetics and confirmed by a continuous experiment. The system is able to generate around 12.2 g product per day.

药物相关支架3,4-dihydro-1 H的合成研究了在连续高温高压盘管反应器中通过Krapcho脱烷氧羰基化反应制得的-1-苯并-2庚因2,5,5-二酮，并将其与分批实验的结果进行了比较。第一步，表征连续反应器的停留时间分布（RTD），然后对批料和连续反应物转化曲线进行初步比较，表明两个反应器之间的转化时间非常吻合。在连续反应器系统中，将反应温度提高到溶剂大气压沸点以上，以增强反应并增加通量。根据批处理动力学估算了在≤3分钟的反应时间内完成原料完全转化的最佳反应参数，并通过连续实验进行了确认。该系统每天可产生约12.2克产品。