对氰基苯甲酰氯

对氰基苯甲酰氯 MSDS

对氰基苯甲酰氯性质、用途与生产工艺

生产方法 

619-65-8

6068-72-0

在磁力搅拌下，将4-氰基苯甲酸（30.00 g，203.90 mmol）分批加入亚硫酰氯（29.11 g，244.68 mmol）中。随后，向反应体系中滴加三滴N,N-二甲基甲酰胺（DMF）作为催化剂。将反应混合物加热至回流状态，持续搅拌1.5小时，反应进程通过薄层色谱（TLC）监测。反应完成后，将溶液在235℃下进行蒸馏，得到白色固体产物对氰基苯甲酰氯，收率为98%（5.50 g），熔点为67.2-68.2°C。产物的结构通过以下表征数据确认：1H NMR（600 MHz，DMSO-d6）δ 8.06（d，J = 7.8 Hz，2H），7.96（d，J = 7.8 Hz，2H）；13C NMR（151 MHz，DMSO-d6）δ 165.9, 134.7, 132.6, 129.9, 118.1, 115.1；IR（KBr，νmax/cm-1）3101, 3051, 2229, 1772, 1739, 1597, 1401, 1287, 1211, 1167, 896, 851, 634；高分辨质谱（HR-MS，ESI）m/z：[M + H]+计算值C8H4ClNO + H+ 166.0053，实测值166.0054。

参考文献：

[1] Patent: US6433211, 2002, B1

[2] Journal of Chemical Research, 2015, vol. 39, # 9, p. 524 - 526

[3] Patent: US6433211, 2002, B1

[4] Patent: CN107226808, 2017, A. Location in patent: Paragraph 0280-0283

[5] Annali di Chimica (Rome, Italy), 1952, vol. 42, p. 94,101

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6068-72-0, 对氰基苯甲酰氯 相关搜索:

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