[H-].[Na+].[N:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][OH:10])[CH:4]=1.Cl[C:12]1[C:13]([NH2:20])=[N:14][C:15]([Cl:19])=[C:16]([Cl:18])[N:17]=1.Cl>COCOC.O>[Cl:18][C:16]1[N:17]=[C:12]([O:10][CH2:9][C:5]2[CH:4]=[N:3][CH:8]=[CH:7][CH:6]=2)[C:13]([NH2:20])=[N:14][C:15]=1[Cl:19]
To a stirred suspension of sodium hydride (1.20 g of a 60% dispersion in oil) in dry dimethoxymethane (40 mL) was added pyridine-3-methanol (2.18 g) in 1,2-dimethoxymethane (10 mL). The resulting suspension was stirred at room temperature for 0.5 h and then 3,5,6-trichloro-2-aminopyrazine (1.2 g) was added and the mixture stirred at 70° C. for 4 h. The reaction mixture was cooled and cautiously added to water (100 mL) and neutralised with 2M hydrochloric acid. The mixture was extracted with ethyl acetate (2×50 mL), dried (MgSO4), filtered and concentrated. The residue was purified by chromatography on silical gel eluting with ethyl acetate to afford the sub-titled compound as a white solid (0.29 g).
読み込み中…
