反应详情

温度

80 °C

To a well stirred solution of step 1 intermediate (200 mg, 0.512 mmol) in ethanol (5 ml) was added NH4Cl (276 mg, 5.102 mmol) in water (3 ml) at room temperature. The reaction mixture was stirred for 15 min at the same temperature and then heated to 80° C. for 15 min. Iron (86 mg, 1.552 mmol) was added at that same temperature. The reaction mixture was refluxed further for 2 h. The residue obtained after the evaporation of the solvent was extracted with chloroform (2×50 ml). This chloroform layer was passed through celite. The layers were separated. Organic layers were washed with water (2×30 ml), brine (30 ml) and dried over Na2SO4. Solvent was evaporated to give 150 mg of the product.

1. temperatureThe reaction mixture was refluxed further for 2 h
2. customThe residue obtained
3. customafter the evaporation of the solvent
4. extractionwas extracted with chloroform (2×50 ml)
5. customThe layers were separated
6. washOrganic layers were washed with water (2×30 ml), brine (30 ml)
7. dry with materialdried over Na2SO4
8. customSolvent was evaporated