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. 6966-01-4, name is Methyl 3-amino-6-bromopyrazine-2-carboxylate, A new synthetic method of this compound is introduced below., 6966-01-4
K2CO3 (0.89 g, 6.46 mmol) was added to a solution of methyl 3-amino-6-bromopyrazine- 2-carboxylate (0.75 g, 3.23 mmol) in anhydrous DME (15 ml) in a pressure tube. Trimethylboroxine (0.99 ml, 3.56 mmol) was added then the resulting brown suspension was de-gassed by bubbling a stream of nitrogen through the reaction mixture for 5 min. Pd(dppf)2C (0.13 g, 0.16 mmol) was added then the pressure tube was flushed with nitrogen and sealed. The reaction was stirred at 100 C for 16 h then allowed to cool to RT. The resulting suspension was filtered then the solid thus obtained was washed with EtOAc (20 ml). The combined filtrate was concentrated in vacuo. The crude material was purified by flash column chromatography on a silica column (50 g). The column was eluted with EtOAc: heptane, increasing the gradient linearly from 0:100 to 50:50 over 10 column volumes. The desired fractions were combined and evaporated to yield the product as a light yellow solid (470 mg, 87%).1H NMR (250 MHz, DMSO-de) delta 8.18 (s, 1 H), 7.11 (s, 2H), 3.83 (s, 3H), 2.33 (s, 3H). LC/MS (System A): m/z (ESI+) = 168 [MH+], Rt = 0.68 min, UV purity = 100%.
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; ENTERPRISE THERAPEUTICS LIMITED; MCCARTHY, Clive; HARGRAVE, Jonathan David; HAY, Duncan Alexander; SCHOFIELD, Thomas Beauregard; WENT, Naomi; (111 pag.)WO2017/221008; (2017); A1;,
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