反应详情

温度

2.5 °C

Compound of example 151 (12 g, 52.1 mmol) was added to 10% aqueous sulfuric acid (110 mL) at 0° C. An aqueous solution (40 mL) of NaNO2 (4.3 g, 62.32 mmol) was added dropwise, with stirring at 0-5° C. The reaction mixture was stirred for 10 min. and was added to an ice cold aqueous solution of copper sulfate (156 g, 1 L, 625 mmol) containing Cu2O (6.8 g, 47.55 mmol). The resultant mixture was stirred at 0° C. for 10 min. It was diluted with water and extracted using EtOAc (3×500 mL). The organic extract was washed with water, dried (anhydrous Na2SO4), concentrated and purified using a silica gel column and 2% EtOAc in petroleum ether (60-80° C.) as eluant to obtain the title compound.

1. stirringThe reaction mixture was stirred for 10 min.
2. extractionextracted
3. extractionThe organic extract
4. washwas washed with water
5. dry with materialdried (anhydrous Na2SO4)
6. concentrationconcentrated
7. custompurified
8. customa silica gel column and 2% EtOAc in petroleum ether (60-80° C.)