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. 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, A new synthetic method of this compound is introduced below., category: Triazoles
In a 500 mL round-bottomed flask, lH-l,2,4-triazole-3,5-diamine (1.5 g, 15.1 mmol, Eq: 1.00) and sodium methoxide 1M (33.3 ml, 16.7 mmol, Eq: 1.1) were combined with MeOH (100 ml) to give a colorless turbid solution. The reaction mixture was stirred for 4 hr and stripped to a gray solid. Suspended in 30 ml DMF and l-(chloromethyl)-4-methoxybenzene (2.42 g, 2.1 ml, 15.4 mmol, Eq: 1.02) was added. The dark brown suspension was stirred at 25C for 60 hrs under argon. The reaction was diluted with water (35 ml) and extracted with EtOAc (3 x 50 ml). The organic layers were combined, washed with H20 (1 x 25 mL), sat NaCl (1 x 50 ml), dried over Na2S04 and concentrated in vacuo to a white pasty solid. Dried under vacuum while gently heating to remove residual DMF and PMB-C1. The crude material was purified by flash chromatography (silica gel, 80g, 0percent to 10percent MeOH in DCM) to give 457 mg of desired product as a yellow solid (14percent). MS (m+1) = 220.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; CHEN, Zhi; CHIN, Elbert; ERICKSON, Shawn David; GABRIEL, Stephen Deems; MERTZ, Eric; WEIKERT, Robert James; WO2014/135483; (2014); A1;,
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