反应详情

温度

70 °C

A stirred solution of 1-chloro-2-(difluoromethyl)-5-fluoro-4-nitrobenzene (D96, 200 mg, 0.89 mmol) in dimethylformamide (4 ml) at room temperature under argon was treated with N,N-diisopropylethylamine (0.47 ml, 2.7 mmol), followed by 1-(tetrahydro-2H-pyran-4-yl)-4-piperidinamine dihydrochloride (D40, 240 mg, 0.94 mmol) and then heated at 70° C. for 1.5 hrs. The reaction 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. This was purified by chromatography on silica gel eluting with 0-20% methanol/ethyl acetate to afford the title compound as a yellow solid (330 mg, 96%).

1. concentrationThe reaction 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
7. customThis was purified by chromatography on silica gel eluting with 0-20% methanol/ethyl acetate