Extracurricular laboratory: Synthetic route of 16298-03-6

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. 16298-03-6, name is Methyl 2-aminopyrazine-3-carboxylate, A new synthetic method of this compound is introduced below., Formula: C6H7N3O2

General procedure: Used for N-benzyl derivatives 1-8. The starting 3-aminopyrazine-2-carboxylic acid(Sigma-Aldrich, Schnelldorf, Germany; 2.2 g; 15.8 mmol) in methanol (250 mL) was cooled downto 0 C and concentrated H2SO4 (3.2 mL) was added. The reaction mixture was stirred for 48 h atrt. Subsequently the reaction mixture was poured into water (27 mL) and alkalized by NaHCO3(approx. 6.3 g) to pH = 7. The precipitate was filtered off and collected as white-brown solid toobtain methyl 3-aminopryzine-2-carboxylate [32]. Methyl 3-aminopyrazine-2-carboxylate (100 mg;0.65 mmol) in methanol (2 mL) along with substituted benzylamine (1.95 mmol; 3 equiv) and NH4Cl(10 mg; 0.19 mmol; 0.1 equiv) [33] were put into reaction tube used for microwave assisted synthesiswith a magnetic stirrer. Reaction was performed in a CEM Discover microwave reactor with a focusedfield in pressurized vials with the following settings: 130 C, 90 W and 40 min. The progress of thereaction was checked using TLC (Merck Silica 60 F254) developed by in hexane/ethyl-acetate 2:1 system.The reaction mixture was adsorbed to silica gel and purified by flash chromatography (Teledyne IscoInc.,) using silica (irregular, 40-63 m) as a stationary phase and gradient elution EtOAc in hexane0-100%, with respect to the expected lipophilicity of the product.

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:
Article; Bouz, Ghada; Semelkova, Lucia; Jand?ourek, Ond?ej; Kone?na, Klara; Paterova, Pavla; Navratilova, Lucie; Kubi?ek, Vladimir; Kune?, Ji?i; Dole?al, Martin; Zitko, Jan; Molecules; vol. 24; 7; (2019);,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem