反应详情

The product from Example 76E (132 mg, 0.26 mmol) in pyridine (5 mL) was treated with O-methylhydroxylamine hydrochloride (26 mg, 0.32 mmol). After stirring for 1 hour at room temperature, the volatiles were evaporated under reduced pressure. The residue was dissolved in ethyl acetate and washed with 1N HCl, water, brine, dried (Na2SO4), filtered and the filtrate concentrated under reduced pressure. The residue was purified by flash chromatography (silica gel, 100:1:1 ethyl acetate:formic acid:water) to provide the title compound as a white solid (43 mg, 31%).

1. customthe volatiles were evaporated under reduced pressure
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed with 1N HCl, water, brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationthe filtrate concentrated under reduced pressure
7. customThe residue was purified by flash chromatography (silica gel, 100:1:1 ethyl acetate:formic acid:water)