Continuously updated synthesis method about 721-63-1

According to the analysis of related databases, 721-63-1, the application of this compound in the production field has become more and more popular.

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 721-63-1 as follows. SDS of cas: 721-63-1

A 100 mL two-necked reaction flask was placed in an ice bath at 0 C, p-trifluoromethylphenylacetate 2i (10.0 mmol) and 20 mL of acetonitrile were added, and p-toluenesulfonyl azide 3a (11.0 mmol) was added.1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) (15.0 mmol) was slowly added.Stir for 5 minutes in an ice bath and place in a microwave reactor.Set power 400W, heating temperature 40 C, heating time 60 min,Turn on the exhaust fan.After the reaction is completed, the mixture is cooled to room temperature, quenched by the addition of ammonium chloride solution, and extracted with dichloromethane and water. The organic phase is collected, dried over anhydrous sodium sulfate, filtered, and evaporated. Chromatography (eluent is petroleum ether (60-90 C) / ethyl acetate, v / v = 80:1),The red solid target product 1i (2.06 g, yield 80%) was obtained.The target product was confirmed by nuclear magnetic resonance spectroscopy and high resolution mass spectrometry.

According to the analysis of related databases, 721-63-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Nanjing Tech University; Gao Zhen; Yi Xiangyan; Huang Fei; Huang He; Yu Yang; Zhang Zhipeng; Xue Lian; Wang Lize; Qiao Nasen; (12 pag.)CN108727216; (2018); A;,
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