反应详情

To a refluxing mixture of hydroxylamine.HCl (2.1 g) in acetic acid (5 cc) was added a solution of 5-benzoyl-2-pentanone (1.9 g) (step 1) in acetic acid (5 cc) and the suspension refluxed for 3 hours. Acetic acid was then removed in vacuo, the residue treated with H2O (25 cc) and extracted with ethyl acetate (3×25 cc); the organic layer was washed with 25% aqueous NH4OAc, dilute NaHCO3 and brine. After removal of the solvent the residue was purified by chromatography to afford the title compound. p.m.r. (CD3CDCD3) δ 7.1-8.2 (m, 8H), 2.55 (s, 3H).

1. temperaturethe suspension refluxed for 3 hours
2. customAcetic acid was then removed in vacuo
3. additionthe residue treated with H2O (25 cc)
4. extractionextracted with ethyl acetate (3×25 cc)
5. washthe organic layer was washed with 25% aqueous NH4OAc, dilute NaHCO3 and brine
6. customAfter removal of the solvent the residue
7. customwas purified by chromatography