化学合成。
化学合成
合成路线 1（1. 合成：2033-42-3）
产率：61%
合成条件：With N-iodo-succinimide; palladium diacetate In N,N-dimethyl-formamide at 80℃; for 3 h; Inert atmosphere; Sealed tube
实验步骤：将2-羟基萘甲酸（37.6mg，0.2mmol），NIS（47.3mg，0.21mmol），乙酸钯（0.9mg，0.002mmol）和搅拌器放入反应管中。 更换惰性气体后，加入1ml溶剂DMF，密封反应管。 将反应管置于80℃的油浴反应器中并搅拌3小时。 冷却至室温后，使用2mol / L氢氧化钠溶液调节pH = 10.将反应管用5ml水稀释并用乙酸乙酯萃取。 合并萃取液，用水洗涤，用硫酸钠干燥，过滤，减压浓缩滤液。 用乙酸乙酯：石油醚= 0至1:30（体积比）洗脱混合物。将粗产物进行柱色谱，得到纯的1-碘-2-萘酚（33.0mg，61％）。
参考文献：
- [1] Patent: CN106748604, 2017, A. Location in patent: Paragraph 0067; 0068
合成路线 2（2. 合成：2033-42-3）
产率：74%
合成条件：With sulfuric acid; dihydrogen peroxide; potassium iodide In methanol at 0 - 20℃;
实验步骤：向搅拌的2-萘酚（1.0g，6.9mmol）和浓盐酸的溶液中加入。 在0℃下，在CH 3 OH（20mL）中的H 2 SO 4（0.54mL，10.4mmol）中加入KI（1.27g，7.62mmol）和30％H 2 O 2（1.56mL，13.9mmol）。 将混合物在室温下搅拌过夜，然后倒入CH 3 Cl中。 将混合物用饱和的水溶液洗涤。 用水洗涤NaHSO 3，用MgSO 4干燥，真空浓缩。 通过快速柱色谱法使用己烷和EtOAc纯化粗产物，得到1-碘-2-萘酚，为浅黄色固体（1.40g，74％），1H NMR（300MHz，CDCl 3）d 7.91（d，J = 8.6Hz） ，1H），7.73-7.70（m，2H），7.53（dd，J = 7.1,8.2 Hz，1H），7.36（dd，J = 7.0,8.1 Hz，1H），7.25-7.23（m，峰值合并， CDCl3，1H），5.79（s，1H）; 13C NMR（75MHz，CDCl3）d 153.7,134.7,130.6,130.2,129.6,128.3,128.1,124.1,116.4,86.2; GC-MS m / z 270,272（M +）。
参考文献：
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