反应详情

温度

75 °C

A stirred suspension of 1-(tetrahydro-2H-pyran-4-yl)-4-piperidinamine dihydrochloride (diHCl salt of D9, 350 mg, 1.4 mmol) in dimethylformamide (6 ml) at room temperature under argon was treated with N,N-diisopropylethylamine 51 mg, 4.0 mmol), then stirred for 10 minutes before adding 2-fluoro-1-nitro-4-[(2,2,2-trifluoroethyl)oxy]benzene (D55, 280 mg, 1.2 mmol) and heating at 75° C. for 36 hrs. The solution was concentrated under vacuum and the residue treated with 10% Na2CO3 solution and extracted with ethyl acetate. The extract was washed with brine, dried (Na2SO4) and concentrated under vacuum. The residue was purified by chromatography on silica gel (20 g) eluting with 0-20% methanol/ethyl acetate to afford the title compound as a bright yellow solid (210 mg, 45%).

1. concentrationThe solution was concentrated under vacuum
2. additionthe residue treated with 10% Na2CO3 solution
3. extractionextracted with ethyl acetate
4. washThe extract was washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated under vacuum
7. customThe residue was purified by chromatography on silica gel (20 g)
8. washeluting with 0-20% methanol/ethyl acetate