反应详情

温度

2.5 °C

Compound of example 156 (9 g, 48.5 mmol) was subjected to diazotization using NaNO2 (4.5 g 48.5 mmol) in water (50 mL) and H2SO4 (10%, 100 mL). Excess nitrous acid was neutralized with urea. The reaction mixture was poured into a suspension of CuSO4.5H2O (144 g, 577 mmol) and Cu2O (5.22 g, 41.4 mmol) in water (900 mL) at 0° C. The reaction mixture was stirred for 15 min. at 0-5° C. and was then extracted using diethyl ether (3×200 mL). The organic extract was washed, dried (anhydrous Na2SO4), concentrated and purified using a silica gel column and 10% EtOAc in petroleum ether (60-80° C.) as eluant to obtain the title compound.

1. extractionwas then extracted
2. extractionThe organic extract
3. washwas washed
4. dry with materialdried (anhydrous Na2SO4)
5. concentrationconcentrated
6. custompurified
7. customa silica gel column and 10% EtOAc in petroleum ether (60-80° C.)