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 6160-65-2 as follows. name: 1,1′-Thiocarbonyldiimidazole
To a stirred solution of 1-Z-piperazine (8.5 g, 38.5 mmol) in dry THE (100 mL), 1,1- thiocarbonyldimidazole (12.37 g, 69.4 mmol) was added and the mixture was stirred at 60C for 5 h. It was concentrated under vacuum and NH3 in EtCH (2 N, 300 mL) was added at 0C. The resulting mixture was stirred at 55C for 8 h in an autoclave. It was diluted withwater (100 mL) and extracted with DCM (2 x 100 mL). The DCM layer was washed with water (100 mL), dried over in anhydrous Na2SO4 and concentrated. The resulting crude product was purified by flash chromatography to afford the title product. Yield: 87% (7 g, white solid). 1H NMR (400 MHz, DMSO-d6): 6 7.51 (5, 2H), 7.38-7.31 (m, 5H), 5.1 (5, 2H), 3.78 (m, 4H), 3.43-3.33 (m, 4H). LCMS: (Method A) 280.2 (M+H), Rt. 2.33 mm, 95.4% (Max).
According to the analysis of related databases, 6160-65-2, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ASCENEURON S. A.; QUATTROPANI, Anna; KULKARNI, Santosh, S.; GIRI, Awadut, Gajendra; (280 pag.)WO2017/144633; (2017); A1;,
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