Synthetic Route of 4774-14-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 4774-14-5 name is 2,6-Dichloropyrazine, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Step 1 To a solution of tert-butyl azetidin-3-ylcarbamate hydrochloride (XLVI) (2 g, 9.58 mmol) in dry DMF (19.2 mL) was added DIPEA (8.37 ml, 47.9 mmol). To this mixture was added 2,6-dichloropyrazine (XLVII) (1.428 g, 9.58 mmol) and the reaction was stirred at 95 C. for 3 hours. The reaction was quenched with water (20 mL) and extracted with EtOAc. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated. The residue was purified by silica gel column chromatography (40 g) (100% hexanes?hexanes:EtOAc 1:1) to yield tert-butyl(1-(6-chloropyrazin-2-yl)azetidin-3-yl)carbamate (XLVIII) (2.2882 g, 8.04 mmol, 84% yield) as a white solid. ESIMS found for C12H17ClN4O2 m/z 285.1 (M+H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,6-Dichloropyrazine, and friends who are interested can also refer to it.
Reference:
Patent; Samumed, LLC; Hood, John; Kumar KC, Sunil; Wallace, David Mark; Mittapalli, Gopi Kumar; Hofilena, Brian Joseph; Mak, Chi Ching; Bollu, Venkataiah; Eastman, Brian; US2015/266825; (2015); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem