Electric Literature of 645-36-3, 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 645-36-3 as follows.
N- (2-chloropyridine-4-substituted) -4-fluorobenzamide (5g, 19.9mmol) was dissolved in toluene (50mL), cooled to 0 C, and dichlorosulfoxide was slowly added dropwise under nitrogen protection. (7.1 g, 59.8 mmol), transferred to room temperature for 1 hour, and then refluxed overnight. TLC monitoring. After the reaction was completed, the solvent and dichlorosulfoxide were removed to obtain (Z) -N- (2-chloropyridine-4-substituted) -4-fluorobenzimidyl chloride.Dissolve aminoacetaldehyde diethanol (3.5 g, 23.9 mmol) and TEA (4.0 g, 39.8 mmol) in dichloromethane (100 mL), cool to 0 C, and obtain (Z) -N- (2-chloropyridine-4-substituted) -4-fluorobenzimidyl chloride was dissolved in dichloromethane (100 mL), and the solution was slowly added dropwise. The mixture was naturally warmed to room temperature and stirred overnight. Monitored by TLC. After the reaction was completed, the mixture was washed with a saturated ammonium chloride aqueous solution and a saturated saline solution, dried over anhydrous Na2SO4, filtered, and dried. Purification by silica gel column chromatography gave a yellow solid (7 g, 95.7%).
According to the analysis of related databases, 645-36-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Southern Medical University; Zhang Jiajie; Yang Haikui; Wu Shaoyu; Tian Yuanxin; Wan Shanhe; Zhang Tingting; Wu Xiaoyun; Li Zhonghuang; Jiang Ying; Yan Ruohong; Zhu Zhengguang; Hu Xiang; (75 pag.)CN110041302; (2019); A;,
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