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用薄层色谱(TLC)跟踪监测合成罗沙替丁醋酸酯过程中每一步反应,结果显示:1—3步的合成反应监测过程采用的展开剂都是甲醇∶氯仿∶氨水(1∶4∶0.5;V/V/V);第4步合成反应监测过程中,当展开剂石油醚∶氯仿∶丙酮∶乙醇的配比为23.5∶12∶2∶2.5(V/V/V/V)时,原料中间体及终产物的Rf值可控制在0.25—0.60之间,并且各物质能够在薄板上很好地分离,罗沙替丁醋酸酯Rf值为0.42,以此作为工业化生产中快速跟踪合成进程的主要检测手段。
The reaction of each step in the synthesis of roxatidine acetate was monitored by thin layer chromatography (TLC). The results showed that the developing reagents used in the synthesis reaction monitoring in 1-3 steps were methanol: chloroform: ammonia (1: 4: 0.5; V / V / V). In the fourth step, when the ratio of petroleum ether: chloroform: acetone: ethanol is 23.5: 12: 2: 2.5 , The Rf value of the raw material intermediate and the final product can be controlled between 0.25-0.60, and each substance can be well separated on the sheet, Ras value of roxatidine acetate is 0.42, so as to be quickly tracked in industrialized production The main means of detection of the synthesis process.