反应详情

5-Nitro-isochromen-1-one (1.2 g, 0.0063 mol) and 40% aqueous methylamine (10 mL, 0.09 mol) were refluxed in methanol (40 mL, 1 mol) for 1 hour. The solvents were removed and the residue was diluted with CH2Cl2/MeOH (95:5 v/v, 100 mL), washed with brine (20 mL×2). The CH2Cl2 layer was dried over Na2SO4, purified via flash chromatography (40 g of silica gel, 0-50% EtOAc/Hexanes) to give a yellow solid. MS m/z (M+H) 204.8.

1. customThe solvents were removed
2. additionthe residue was diluted with CH2Cl2/MeOH (95:5 v/v, 100 mL)
3. washwashed with brine (20 mL×2)
4. dry with materialThe CH2Cl2 layer was dried over Na2SO4
5. custompurified via flash chromatography (40 g of silica gel, 0-50% EtOAc/Hexanes)
6. customto give a yellow solid