反应详情

温度

120 °C

Based on the method described in WO2004/052869, mercaptoethanol (0.93 mL) and tetrakis(triphenylphosphine)palladium (3.39 g) were added to a solution of 1.00 g of 2-amino-5-bromopyrazine (5.75 mmol) in N,N-dimethylformamide (15.1 mL), and the resulting mixture was heated and stirred in a sealed tube for about 3 hours at 120° C. After cooling, the reaction mixture was diluted with water, and then extracted (100 mL×6) with a mixed liquid (methylene chloride:ethanol=5:1). The organic layer was dried over anhydrous sodium sulfate, then filtered, and the solvent was removed by distillation under reduced pressure. The resulting residue was purified by column chromatography (hexane:ethyl acetate=1:1, then ethyl acetate, and then ethyl acetate:methanol=10:1), then recrystallized (chloroform) to obtain 470 mg of the title compound (yield 44%) as yellow needle-like crystals.

1. temperaturethe resulting mixture was heated
2. temperatureAfter cooling
3. extractionextracted (100 mL×6) with a mixed liquid (methylene chloride:ethanol=5:1)
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. customthe solvent was removed by distillation under reduced pressure
7. customThe resulting residue was purified by column chromatography (hexane
8. customethyl acetate=1:1, then ethyl acetate, and then ethyl acetate:methanol=10:1), then recrystallized (chloroform)