Hydrochloric Acid → HCID 54388748, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1.41 g of the acid of Step A, 4.5 g of 0-tert.-butyl-N,N-diisopropyl-isourea and 32 ml of tetrahydrofuran was stirred at 20° C. under nitrogen for 15 hours and then 8 ml of aqueous N hydrochloric acid were added with stirring. 8 ml of aqueous N sodium hydroxide solution and 10 ml of ether were added with stirring and the mixture was filtered. The decanted aqueous phase was extracted with ether and the combined organic phases were washed and evaporated to dryness under reduced pressure. The residue was chromatographed over silica and was eluted with a 93-7 methylene chloride-acetone mixture to obtain 1.35 g of 1,1-dimethyl-ethyl 2-oxo-4-{pyridin-3-yl)-3-butenoate melting at 51°-52° C.

Provenance & Evidence