6340-79-0 3-(4-溴苯甲酰基)丙酸

危险性质：非危险化学品

化学合成。

化学合成

合成路线 1（1. 合成：6340-79-0）

产率：93.4% 合成条件：Stage #1: at 0 - 20℃; for 100 h; Inert atmosphere Stage #2: at 0℃; for 1 h; Inert atmosphere 实验步骤：将琥珀酸酐3（5.0g，50mmol）和溴苯2（48g，300mmol）冷却至0℃。加入氯化铝（13.3g，100mmol）并将混合物在0℃和氮气氛下搅拌4小时。使反应温热至室温并在氮气氛下搅拌96小时。将反应冷却至0℃并加入浓HCl（125mL）并将反应在氮气下再搅拌1小时。过滤反应物并用水（1L）洗涤，得到浅黄色固体，将其从甲苯中重结晶，得到4-（4-溴苯基）-4-氧代丁酸4（12g，46.68mmol，93.4％）。 MS（ESI-QUADRUPOLE）m / z：计算值。对于Ci0H9BrO3：255.97,257.97;实测值：258.0（11），257.0（98），256.0（12），255.0（100），213.0（18），21.1.0（17）（负离子）。 HPLC：tr = 24.4min 1 H NMR（500MHz，ofe-DMSO）δ：2.59（2H，t，J = 6.5Hz，CH2），3.21（2H，t，J = 6.5Hz，CH2），7.88 （2 H，d，J = 8.8Hz，ArH），7.96（2H，d，J = 8.8Hz，ArH），12.19（1H，br s，OH）。 参考文献：

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