反应详情

Iron powder (265 mg, 4.7 mmol), ammonium chloride (35 mg, 0.65 mmol) and the nitroindane from Step 7 (275 mg, 0.82 mmol) were mixed together in ethanol (5 ml) and water (2.5 mL). The mixture was refluxed for l h and then filtered through celite, washing the cake with EtOAc. The volatile, s were removed in vacuo and the residue was dissolved in EtOAc:CH2Cl2 (3:1), washed with brine and dried over MgSO4. Evaporation of the solvent left a residue that was purified by flash chromatography on silica gel (EtOAc:toluene:CH2Cl2 from 30:50:20 to 1:1:1 ) to give 150 mg of the title compound.

1. temperatureThe mixture was refluxed for l h
2. filtrationfiltered through celite
3. washwashing the cake with EtOAc
4. customThe volatile, s were removed in vacuo
5. dissolutionthe residue was dissolved in EtOAc:CH2Cl2 (3:1)
6. washwashed with brine
7. dry with materialdried over MgSO4
8. customEvaporation of the solvent
9. waitleft a residue that
10. customwas purified by flash chromatography on silica gel (EtOAc:toluene:CH2Cl2 from 30:50:20 to 1:1:1 )