Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 16461-94-2, name is 4-Bromo-1H-pyrazol-3-amine, A new synthetic method of this compound is introduced below., COA of Formula: C3H4BrN3
Experimental steps: Weigh AsB-COOH (67.4 mg, 0.142 mmol, 1 eq) in a 50 ml round bottom flask.The compound was dissolved in 2 ml of anhydrous 1,2-dichloroethane, and then EDC (57.2 mg, 0.298 mmol, 2 eq) was weighed.HoBt (75.2 mg, 0.5565 mmol, 4 eq) was reacted in the reaction mixture for 4 h at room temperature.The reamine (0.3 mmol, 2 eq) was refluxed at 80 C for 12 h, and the reaction was followed by TLC.After the completion of the reaction, the solvent was evaporated under reduced pressure at room temperature, and extracted with 0.5 M HCl and EA (V: V = 1:1) to obtain an organic phase (50 ml of a separating funnel).The obtained organic phase was transferred to a 125 ml separatory funnel, followed by saturated brine (2×20 ml), 5% sodium hydrogen carbonate solution (2×20 ml).Saturated saline solution (3 × 20 ml) was added, and the pH of the saturated saline solution extracted at the end was measured, and the pH was neutral.The organic phase was dried over anhydrous sodium sulfate, and the crude product was evaporated under reduced pressure at 45 C. White soldi, yiled 60.5%
The synthetic route of 16461-94-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; South China Normal University; Long Yuhua; Li Tingmei; She Zhigang; Fan Weilong; Wen Shitong; Yan Zhangyuan; Guo Huixian; Huang Cuiying; Jiang Lasheng; (32 pag.)CN108191944; (2018); A;,
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