Synthetic Route of 450-91-9, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 450-91-9 as follows.
Under an ice bath condition, 4-fluoro-2-methoxyaniline (Intermediate 102) (15 g, 106.4 mmol, 1.0 eq) was added dropwise to a concentrated sulfuric acid (150 mL) while controlling the temperature around 0C during the course of addition. After the forming solid was dissolved completely, potassium nitrate (11 g, 106.4 mmol, 1.0 eq) was added portionwise and the reaction was continued for 1 hour under this condition. The reaction was poured into ice water and the pH was adjusted to basic by sodium hydroxide. A vast amount of solid was precipitated out which was filtered and washed with water, petroleum ether, dried in air to give 4-fluoro-2-methoxy-5-nitroaniline as a brown solid (18 g, yield: 77%). LCMS (ESI): m/z 187 [M + H]+.
According to the analysis of related databases, 450-91-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Guangzhou Bebetter Medicine Technology Co., Ltd.; CAI, Xiong; QIAN, Changgeng; WENG, Yunwo; LIU, Bin; WANG, Yanyan; LIN, Mingsheng; LI, Junqi; QING, Yuanhui; YOU, Huajin; ZHOU, Shiqing; XUE, Weicai; (76 pag.)EP3345900; (2018); A1;,
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