化学合成。
化学合成
合成路线 1（1. 合成：26260-02-6）
产率：83%
合成条件：With perfluoroisopropyl iodide; copper; hydroquinone In N,N-dimethyl-formamide at 20℃; for 24 h;
实验步骤：通用方法：将（4-硝基苯基）硼酸（0.067g，0.4mmol），铜粉（0.0052g，0.08mmol），（CF3）2 CFI（0.178g，0.6mmol）和DMF（2mL）置于 一个带橡胶塞的封闭管。 将混合物在室温下与气球反应24小时。 将所得悬浮液倒入水中并用乙酸乙酯萃取。 将有机层用无水Na 2 SO 4干燥并浓缩至干。 通过硅胶快速柱色谱法纯化粗产物，使用石油醚/乙酸乙酯= 20：1（v / v）作为洗脱剂，得到0.086g 2j，为浅黄色固体（0.35mmol，87％）。
参考文献：
- [1] Journal of Fluorine Chemistry, 2016, vol. 189, p. 59 - 67
合成路线 2（2. 合成：26260-02-6）
产率：98%
合成条件：With silica gel; pyridinium chlorochromate In dichloromethane at 20℃; Inert atmosphere
实验步骤：将PCC（415mg，1.93mmol，1.2当量）和硅藻土（1.75g）在2颈烧瓶中真空干燥，然后用氮气冲洗。 在19.3mL无水DCM中悬浮后，在室温下逐滴加入邻 - 碘代苄醇（14）（390mg，1.60mmol，1.0当量）在无水DCM（5.33mL）中的溶液。 反应混合物从红色变为棕色，然后变为黑色，并在环境温度下搅拌过夜。 通过硅藻土过滤后，减压除去溶剂。 通过快速色谱法（短柱，洗脱液己烷/ EtOAc = 9/1）纯化粗残余物，得到367mg（98％）醛15.（R）（己烷/ EtOAc = 9/1）= 0.63; 1H NMR（400MHz，CDCl3）δ（ppm）= 10.1（1H，s，H-7），7.97（1H，dd，H-3，J = 8.0,1.0Hz），7.87（1H，dd，H-6） ，J = 8.0,1.8Hz），7.42-7.48（1H，m，H-4），7.25-7.31（1H，m，H-5）; 13C NMR（101MHz，CDCl3）δ（ppm）= 195.9（C-7），140.8（C-4），135.6（C-3），135.3（C-1），130.4（C-5），128.9（C） -6），100.9（C-2）。
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