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地西泮的合成工艺优化研究

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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。
Optimizationon of the Synthesis Process of Diazepam
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)