反应详情

3-amino-6-bromo-pyrazine-2-carboxamide (500 mg, 2.304 mmol) was dissolved in pyridine (5 mL) and treated with POCl3 (666 μL, 7.145 mmol) dropwise at 0° C. After the addition was complete the reaction was allowed to warm to ambient temperature and stirred for 1.5 hours. The solvent was removed in vacuo and the reaction carefully treated with NaHCO3 to basify. The mixture was diluted with EtOAc and the layers separated. The aqueous layer was further extracted with EtOAc (1×) and the combined organics washed with brine (1×), 0.1 M HCl (1×) and water (1×), dried (MgSO4), filtered and concentrated to furnish the product as a brown solid (197 mg, 43% Yield). 1H NMR (DMSO) d 7.62 (2H, br s), 8.45 (1H, s) ppm

1. additionAfter the addition
2. customThe solvent was removed in vacuo
3. customthe reaction
4. customthe layers separated
5. extractionThe aqueous layer was further extracted with EtOAc (1×)
6. washthe combined organics washed with brine (1×), 0.1 M HCl (1×) and water (1×)
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated