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ChemicalBook CAS DataBase List Thidiazuron
51707-55-2

Thidiazuron synthesis

2synthesis methods
-

Yield:51707-55-2 70%

Reaction Conditions:

with selenium;oxygen;triethylamine in N,N-dimethyl-formamide at 100; for 8 h;Catalytic behavior;Reagent/catalyst;Solvent;Temperature;

Steps:

General procedure for the selenium-catalyzed oxidative carbonylation reaction
General procedure: General procedure for the selenium-catalyzed oxidative carbonylation reaction: Selenium (0.1 mmol, 0.05 equiv.), 1,2,3-thiadiazol-5-amine (2 mmol, 1 equiv.), amine (2 mmol, 1 equiv.), Et3N (2 mmol, 1 equiv.), DMF (5 mL) were charged in a 50 mL round-bottom flask equipped with stir bar. Then the flask was evacuated and back-filled three times with CO/O 2 (9:1, balloon) and bubbled with stirring at 100 °C for 8 h. Upon the completion of reaction, the mixture was cooled to room temperature and vented to discharge the excess balloon gas, followed by stirring for 30 min in the atmosphere to precipitate Se adequately, which was collected by suction filtration. Subsequently, the filtrate was concentrated and the residue was purified by column chromatography (silica gel, petroleum ether-ethyl acetate, 3:1) to afford the desired products.

References:

Zhang, Xiaopeng;Dong, Shuxiang;Ding, Qianqian;Fan, Xuesen;Zhang, Guisheng [Chinese Chemical Letters,2019,p. 375 - 378] Location in patent:supporting information

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