反应详情

Acetophenone 12 (50 mg, 0.301 mmol) was condensed with O-(3-fluorobenzyl)hydroxylamine hydrochloride (26) (59 mg, 0.332 mmol) according to the general procedure II-B defined above. After being heated at reflux for 48 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 CP30262 (71 mg, 82%) as a pale-pink oil, Rf 0.6 in 1:1 v/v ethyl acetate/hexane.

1. temperatureAfter being heated
2. temperatureat reflux for 48 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. washwashed with H2O (2×10 mL)
7. dry with materialthen dried (MgSO4)
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe oil thus obtained
11. washwas subjected to flash chromatography (1:19 v/v ethyl acetate/hexane elution)