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. 4923-01-7, name is 5-Methyl-4H-1,2,4-triazol-3-amine, A new synthetic method of this compound is introduced below., name: 5-Methyl-4H-1,2,4-triazol-3-amine
Example 20A (rac)-Ethyl 7-(4-cyanophenyl)-2,5-dimethyl-4,7-dihydro[1,2,4]triazolo[1,5-a]pyrimidine-6-carboxylate Under an atmosphere of argon, ethyl 2-(4-cyanobenzylidene)-3-oxobutanoate (381 mg, 1.6 mmol) and 5-methyl-4H-1,2,4-triazole-3-amine (200 mg, 2.0 mmol, 1.3 eq.) were dissolved in DMF (4 ml), and solid sodium bicarbonate (659 mg, 7.8 mmol, 5 eq.) was added. The mixture was stirred at 65 C. for 12 h. The mixture was then filtered, and the DMF from the filtrate was distilled off under reduced pressure. The residue was purified by preparative HPLC (Gromsil C18 column, 30*250 mm; mobile phase: acetonitrile-water-0.1% TFA). After lyophilization, the product was obtained as a solid (300 mg, 46% of theory). LC-MS (Method 2): Rt=1.92 min; MS (ESIpos): m/z (%)=324.1 (100) [M+H]+; MS (ESIneg): m/z (%)=322.1 (100) [M-H]-. 1H-NMR (400 MHz, DMSO-d6): delta=1.0 (t, 3H), 2.1 (t, 3H), 2.4 (s, 3H), 3.4 (m, 2H), 6.25 (s, 1H), 7.4 (m, 2H), 7.8 (m, 2H), 10.75 (s, 1H).
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; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; US2012/4203; (2012); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics