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对氯苯肼盐酸盐的相转移催化合成工艺研究

Synthesis of p-chlorophenylhydrazine hydrochloride with phase transfer catalysis
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摘要 以对氯苯胺为原料,经相转移催化、还原和水解反应得到目标产物对氯苯肼盐酸盐,其结构经^(1)H-NMR和ESI-MS表征确认,并重点优化了相转移催化阶段对氯苯肼盐酸盐的合成工艺。在相转移催化阶段,适宜的反应条件为:以β-环糊精(β-CD)为相转移催化剂,乙酸为助溶剂,物料比n(HCl):n(NaNO_(2)):n(对氯苯胺)=2.2:1.4:1.0,β-CD的质量用量为3%(以对氯苯胺为基准计),反应温度为25℃。在该优化反应条件下,对氯苯肼盐酸盐的收率为95.46%(以对氯苯胺为基准计算)。 The synthesis of chlorophenylhydrazine hydrochloride was reported.The target compounds were synthesized through phase transfer catalyst reaction,reduction reaction and hydrolysis reaction by using the readily available materials of p-chloroaniline.The ^(1)H-NMR and ESI-MS were used to characteristic the structures of target compounds.Moreover,The synthesis process in the phase transfer catalyst reaction was studied and the suitable reaction conditions were determined as follows:the phase transfer catalyst was beta-cyclodextrin(β-CD);the acetic acid was used as cosolvent;material ratio n(HCl):n(NaNO_(2)):n(p-chloroaniline)=2.2:1.4:1.0;the dosage ofβ-CD was 3%(calculated based on p-chloroaniline);the reaction temperature was 25℃.Under the above conditions,the yield of the product was up to 95.46%(calculated based on p-chloroaniline).
作者 张健楠 袁旭力 殷思佳 李佳盈 熊天健 唐文强 ZHANG Jian-nan;YUAN Xu-li;YIN Si-jia;LI Jia-ying;XIONG Tian-jian;TANG Wen-qiang(School of Pharmacy,Shaanxi Institute of International Trade&Commerce,Xianyang 712046,China)
出处 《精细与专用化学品》 CAS 2023年第6期46-50,共5页 Fine and Specialty Chemicals
基金 2022年国家级大学生创新创业训练计划项目(S202213123005) 咸阳市分子影像与药物合成重点实验室项目(2021QXNL-PT-0008)。
关键词 对氯苯胺 对氯苯肼盐酸盐 相转移催化 合成 p-chloroaniline p-chlorophenylhydrazine hydrochloride phase transfer catalyst synthesis
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