Analyzing the synthesis route of 3,5-Dibromo-1-methylpyrazin-2(1H)-one

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.

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. 87486-34-8, name is 3,5-Dibromo-1-methylpyrazin-2(1H)-one, A new synthetic method of this compound is introduced below., Quality Control of 3,5-Dibromo-1-methylpyrazin-2(1H)-one

A 100-mL three-neck round-bottomed flask equipped with a reflux condenser, magnetic stirrer and nitrogen inlet was charged with 116b (400 mg, 1.66 mmol), 3,5- dibromo-1 -methyl pyrazin-2(lH)-one (443 mg, 1.66 mmol), cesium carbonate (1.19 g, 3.65 mmol), and 1,4-dioxane (20 mL). After bubbling nitrogen through the resulting suspension for 30 min, Xantphos (144 mg, 0.249 mmol) and tris(dibenzylideneacetone)-dipalladium(0) (152 mg, 0.166 mmol) were added, and the reaction mixture was heated at reflux for 4 h. After this time, the mixture was cooled to room temperature and filtered, and the filter cake was washed with methylene chloride (2 x 20 mL). The filtrates were combined and concentrated under reduced pressure, and the resulting residue was purified by column chromatography to afford a 51percent yield (353 mg) of 116c as a yellow solid: mp 172-173 °C; ]H NMR (500 MHz, CDC13) delta 8.17 (s, 1H), 8.06 (s, 1H), 7.65 (s, 1H), 6.70 (s, 1H), 4.28 (t, 2H, / = 5.0 Hz), 3.97 (t, 2H, / = 5.5 Hz), 3.51 (s, 3H), 0.85 (s, 9H), -0.79 (s, 6H); MS (APCI+) m/z 428.3 (M+H).

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.