反应详情

温度

90 °C

A mixture of 2-amino-3-nitro-6-(3-trifluoromethyl-piperidin-1-yl)benzonitrile (200 mg, 0.64 mmol), Fe (178 mg, 3.18 mmol), aqueous NH4Cl (5 mL) and EtOH (5 mL) was heated under Ar at 90° C. for 2 h. The mixture was thereafter basicified to pH ˜9-10 and filtered through celite and the celite pad was washed with EtOH and EtOAc. The organic layer was concentrated and the residue was extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was washed with Et2O to give the sub-title compound.

1. filtrationfiltered through celite
2. washthe celite pad was washed with EtOH and EtOAc
3. concentrationThe organic layer was concentrated
4. extractionthe residue was extracted with EtOAc
5. dry with materialThe organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. washThe residue was washed with Et2O