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地西泮的合成工艺优化研究

Optimizationon of the Synthesis Process of Diazepam

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在地西泮的合成研究中,分别对碳酸氢铵、碳酸铵和HA这三种环合剂做了比较,通过实验发现,碳酸氢铵环合剂在地西泮合成中效果和收率较好.在进一步实验中通过调整2-(N-甲基氯乙酰氨)-5-氯二苯甲酮和碳酸氢铵的物质量比、反应温度和反应时间,找到最佳的合成条件.结果表明,反应温度为52℃,反应时间为7h,对地西泮的合成产率有着显著的影响,当2-(N-甲基氯乙酰氨)-5-氯二苯甲酮和碳酸氢铵的物质量比为1∶6时,地西泮的合成收率最高.在结果可靠性验证实验中,进行了三次重复实验,合成收率分别为84.8%、84.7%和84.9%,进一步表明在该工艺条件下,合成地西泮收率是相对稳定和可靠的.
In the synthesis of diazepam,ammonium bicarbonate,ammonium carbonate and HA were compared respectively,and the effect and yield of ammonium bicarbonate cyclic in diazepam synthesis were better.In further experiments,the optimal syn-thesis conditions were found by adjusting the mass ratio,reaction temperature and reaction time of 2-(N-methyl-chloroacetamide)-5-chlorobenzbenone and ammonium bicarbonate.The results showed that the reaction temperature of 52℃and the reaction time of 7 h had a significant effect on the synthesis yield of diazepam,with the highest mass yield of diazepam when 2-(N-methyl-chloro-acetyl)-5-chlorophenone and ammonium bicarbonate was 1∶6.In the resulting reliability validation experiment,three replicate ex-periments were performed with synthetic yields of 84.8%,84.7%and 84.9%,which further showed that the yield of synthetic diaze-pam was relatively stable and reliable under this process condition.

diazepam2-(N-Methyl chloroacetamide)-5-Methyl chlorideammonium bicarbonate

张健

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山西大同大学化学与化工学院,山西大同 037009

地西泮 2-(N-甲基氯乙酰氨)-5-氯二苯甲酮 碳酸氢铵

2024

山西大同大学学报(自然科学版)
山西大同大学

山西大同大学学报(自然科学版)

影响因子:0.271
ISSN:1674-0874
年,卷(期):2024.40(3)