反应详情

Fe powder (631 mg, 11.3 mmol) was added to a solution of 2,6-dichloro-N-cyclobutyl-5-nitropyrimidin-4-amine (crude, 5.65 mmol) in HOAc (5 mL) and the mixture was stirred at rt for 30 min. The mixture was filtered through Celite® and the volatiles were removed under reduced pressure. The resulting residue was diluted with EtOAc (80 mL) and washed with water (80 mL), sat. NaHCO3 (80 mL) and brine (80 mL). The organic layer was dried over Na2SO4 and concentrated to give the title compound as a brown oil which was used without purification. m/z (APCI+) for C8H10Cl2N4 233.15/235.10 (M+H)+.

1. filtrationThe mixture was filtered through Celite®
2. customthe volatiles were removed under reduced pressure
3. additionThe resulting residue was diluted with EtOAc (80 mL)
4. washwashed with water (80 mL), sat. NaHCO3 (80 mL) and brine (80 mL)
5. dry with materialThe organic layer was dried over Na2SO4
6. concentrationconcentrated