202197-26-0, A common heterocyclic compound, 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline, molecular formula is C13H11ClFNO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A 100-ml three-necked round bottom flask was charged with 15 ml of water, At 0 deg C (0.45 g, 1.81 mmol) 3-chloro-4- (3-fluorobenzyloxy)aniline and NaNO2 (0.25 g, 3.62 mmol) were successively added with stirring, HCl (0.19 g, 5.42 mmol) was added dropwise, Speed can not be too fast, After completion of the dropwise addition, The temperature of the reaction system was maintained at 0-5 deg C for 1.5 h. The color of the reaction liquid was deepened. An aqueous solution of NaN3 (0.14 g, 2.17 mmol) was then added, Must be added and the speed can not be too fast, During the addition, a large amount of foam is generated, Reaction solvent water is added at this time. After completion of the addition, the reaction was continued for 3 h while the temperature was kept constant, and the progress of the reaction was monitored by TLC during the reaction. During the course of the reaction, the color of the reaction solution was found to change from dark yellow to light yellow with yellow foam. At the end of the reaction, The reaction solution was extracted with EA (3 * 40 ml)The organic phase was washed with brine (3 * 10 ml) The organic phases were combined, Mg2SO4 concentrate, Purification by silica gel column chromatography gave 0.48 g (yield: 95.05%) of a yellow solid.
The synthetic route of 202197-26-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Tianjin International Joint Academy of Biotechnology & Medicine; Chen, Yue; Rao, Zihe; Yang, Cheng; Bai, Cuigai; Zhang, Wei; Pan, Chengwen; Meng, Fanfei; Wang, Song; (11 pag.)CN103159748; (2016); B;,
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