反应详情

温度

120 °C

A mixture of 4-(benzyloxy)aniline (2.26 g), 2-chloro-5-fluoro-3-nitropyridine (2 g) and K2CO3 (3.13 g) in DMF (20 mL) was stirred at 120° C. for 5 h, treated with water, and extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated in vacuo. The residue was suspended in IPE and collected by filtration. The obtained solid was dissolved in EtOH (20 mL), and Pt/C (2 g) was added. Under H2 atmosphere, the mixture was stirred for 1 h, filtered and evaporated. The residue was chromatographed on silica gel eluting with Hexane/AcOEt to give the title compound (0.85 g).

1. extractionextracted with AcOEt
2. dry with materialThe organic layer was dried over MgSO4
3. concentrationconcentrated in vacuo
4. filtrationcollected by filtration
5. dissolutionThe obtained solid was dissolved in EtOH (20 mL)
6. additionPt/C (2 g) was added
7. stirringUnder H2 atmosphere, the mixture was stirred for 1 h
8. filtrationfiltered
9. customevaporated
10. customThe residue was chromatographed on silica gel eluting with Hexane/AcOEt