反应详情

The crude nitronaphthyl-pyrimidinyl ether from above (459 mg, 1.42 mmol, 1 equiv.) was taken up in 35 mL EtOAc and 35 mL EtOH. Ammonium formate was added (537 mg, 8.52 mmol, 6 equiv.) as well as 400 mg of 10% palladium-on-carbon. The reaction mixture was heated to a gentle reflux for one h, cooled back to room temperature, filtered through diatomaceous earth and the volatiles were removed in vacuo. The crude product was purified by chromatography on SiO2, eluting with 20-40% EtOAc in hexanes. The desired aminonaphthyl-pyrimidinyl ether was isolated as a yellow foam (176 mg, 0.6 mmol, 42% for 2 steps).

1. temperatureThe reaction mixture was heated to
2. temperaturea gentle reflux for one h
3. filtrationfiltered through diatomaceous earth
4. customthe volatiles were removed in vacuo
5. customThe crude product was purified by chromatography on SiO2
6. washeluting with 20-40% EtOAc in hexanes