Synthetic Route of 774608-89-8, 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 774608-89-8 as follows.
Ethyl 5-bromo-2H-1 ,2,4-triazole-3-carboxylate (Hechung Huaxue, 2004, 12(2), 191-193, Chem. Abs. 141 :350095) (3.11 g, 14 mmol) was dissolved in methanol (50 ml) and cooled to 0 0C. Trimethylsilyl diazomethane (-14 ml of a 2 M solution in ether) was added until a pale yellow colour persisted and the reaction was warmed to room temperature and quenched by the addition of excess acetic acid. It was then evaporated and the residue was partitioned between ethyl acetate and saturated sodium bicarbonate. The organic extract was dried, filtered and evaporated to yield a residue which was purified and separated into its three isomers by silica chromatography using ethyl acetate / petrol. Isomer A (least polar) (1.2 g, 5.1 mmol). 1H NMR (DMSO) delta 4.36 (2 H, q, J = 7 Hz), 4.10 (3 H, s), 1.32 (3 H, t, J=V Hz)Isomer B (medium polarity) (0.47 g, 2.0 mmol). 1H NMR (DMSO) 64.31 (2 H, q, J = 7 Hz), 3.92 (3 H, s), 1.29 (3 H, t, J = 7 Hz) Isomer C (most polar) (0.37 g, 1.6 mmol). 1H NMR (DMSO) 54.38 (2 H, q, J = 7 Hz), 3.82 (3 H, s), 1.33 (3 H, t, J = 7 Hz) Combined yield 62 %.
According to the analysis of related databases, 774608-89-8, the application of this compound in the production field has become more and more popular.
Reference:
Patent; PARADIGM THERAPEUTICS LTD.; WO2007/582; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics