反应详情

Acetophenone 12 (50 mg, 0.301 mmol) was condensed with O-(3-methylbenzyl)hydroxylamine hydrochloride (28) (57 mg, 0.328 mmol) according to the general procedure II-B defined above. After being heated for 15 h the reaction mixture was cooled and the solvent removed under reduced pressure. The ensuing residue was dissolved in CH2Cl2 (15 mL), washed with H2O (2×10 mL) then dried (MgSO4), filtered and concentrated under reduced pressure. The oil thus obtained was subjected to flash chromatography (1:19 v/v ethyl acetate/hexane elution) to afford the title compound CP30264 (78 mg, 91%) as a pale-orange oil, Rf 0.6 in 1:1 v/v ethyl acetate/hexane.

1. temperatureAfter being heated for 15 h the reaction mixture
2. temperaturewas cooled
3. customthe solvent removed under reduced pressure
4. dissolutionThe ensuing residue was dissolved in CH2Cl2 (15 mL)
5. washwashed with H2O (2×10 mL)
6. dry with materialthen dried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe oil thus obtained
10. washwas subjected to flash chromatography (1:19 v/v ethyl acetate/hexane elution)