反应详情

温度

70 °C

A stirred solution of 1-bromo-5-fluoro-4-nitro-2-(trifluoromethyl)benzene (D53) (0.30 g, 1.04 mmole) in dimethylformamide (5 ml) at room temperature under argon was treated with diisopropylethylamine (0.59 ml, 3.3 mmole) and 1-(tetrahydro-2H-pyran-4-yl)-4-piperidinamine dihydrochloride (D40) (0.28 g, 1.1 mmole) and heated at 70° C. for 1 hr. The mixture was concentrated under vacuum and the residue treated with 10% Na2CO3 solution and extracted with ethyl acetate. The extract was dried and concentrated under vacuum to leave an orange solid which was purified by chromatography on silica gel eluting with 0-20% methanol/ethyl acetate to afford the title compound as a bright yellow solid (0.38 g, 81%). MH+=452, 454.

1. concentrationThe mixture was concentrated under vacuum
2. additionthe residue treated with 10% Na2CO3 solution
3. extractionextracted with ethyl acetate
4. customThe extract was dried
5. concentrationconcentrated under vacuum
6. customto leave an orange solid which
7. customwas purified by chromatography on silica gel eluting with 0-20% methanol/ethyl acetate