Sulfuric Acid → HCID 178501905, compound

Participants

Reaction Steps

(RS)-1-Methoxycarbonyl-4-oxo-5-methylpiperidine-3-carbohydroxamic acid ethylene ketal (3.95 g; 14.4 mmol) was at 5° C. added in small portions to a mixture of 96% H2SO4 (9 ml) and water (1 ml). The mixture was then kept at 50° C. for 30 min. and poured on ice. The pH was adjusted to 3 with 9N sodium hydroxide and the mixture was extracted three times with methylene chloride (75 ml). Evaporation in vacuo yielded 2.23 g of crude product. To obtain an analytically pure sample the crude product was purified by CC (eluent: ethyl acetate containing 2% methanol and 2% glacial acetic acid). Recrystallization from toluene yielded the pure title compound, M.P. 128°-129° C.

Provenance & Evidence