反应详情

Acetophenone 12 (50 mg, 0.301 mmol) was condensed with O-(4-carbomethoxybenzyl)hydroxylamine hydrochloride (27) (72 mg, 0.331 mmol) according to the general procedure II-B defined above. After being heated at reflux for 15 h the reaction mixture was cooled and the solvent removed under reduced pressure. The ensuing residue was dissolved in CH2Cl2 (15 mL) and the resulting solution washed with H2O (2×10 mL) then dried (MgSO4), filtered and concentrated under reduced pressure. The residue thus obtained was subjected to flash chromatography (1:9 v/v ethyl acetate/hexane elution) to afford the title compound CP30263 (71 mg, 82%) as a white solid, m.p. 97.7-98.7° C., Rf 0.5 in 1:1 v/v ethyl acetate/hexane.

1. temperatureAfter being heated
2. temperatureat reflux for 15 h the reaction mixture
3. temperaturewas cooled
4. customthe solvent removed under reduced pressure
5. dissolutionThe ensuing residue was dissolved in CH2Cl2 (15 mL)
6. washthe resulting solution washed with H2O (2×10 mL)
7. dry with materialthen dried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe residue thus obtained
11. washwas subjected to flash chromatography (1:9 v/v ethyl acetate/hexane elution)