4-氯苯甲酰肼性質(zhì)、用途與生產(chǎn)工藝

生產(chǎn)方法 

7335-27-5

536-40-3

以對(duì)氯苯甲酸乙酯為原料合成4-氯苯甲酰肼的一般步驟：采用一鍋法常規(guī)合成酰肼（產(chǎn)率30-58%）。將10 mmol對(duì)氯苯甲酸乙酯溶于20 mL乙醇中。向溶液中加入2 mL 3N硫酸，并將反應(yīng)混合物回流6小時(shí)。反應(yīng)進(jìn)程通過(guò)薄層色譜（TLC）監(jiān)測(cè)。反應(yīng)完成后，用固體NaHCO3中和反應(yīng)混合物，過(guò)濾去除過(guò)量的NaHCO3。在中和后的反應(yīng)混合物中，加入1.5 mL（3 mmol）一水合肼，繼續(xù)回流3-6小時(shí)以確保反應(yīng)完全。通過(guò)蒸餾將乙醇和未反應(yīng)的肼蒸發(fā)至原體積的1/3。將反應(yīng)混合物冷卻至室溫，過(guò)濾收集產(chǎn)物，并用甲醇重結(jié)晶，得到純凈的4-氯苯甲酰肼晶體（具體數(shù)據(jù)參見(jiàn)支持信息）。

參考文獻(xiàn)：

[1] Medicinal Chemistry Research, 2013, vol. 22, # 6, p. 2755 - 2767

[2] Bioorganic and Medicinal Chemistry, 2015, vol. 23, # 17, p. 6014 - 6024

[3] Patent: CN106008390, 2016, A. Location in patent: Paragraph 0015

[4] Journal of Heterocyclic Chemistry, 1992, vol. 29, # 5, p. 1101 - 1109

[5] Oriental Journal of Chemistry, 2017, vol. 33, # 2, p. 971 - 978

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