Ethanol → HCID 178469035, compound

Participants

Reaction Steps

A mixture of the product of Stage (i) in absolute ethanol (16 ml) and methylamine in ethanol (33% w/w 8 ml) was stirred at room temperature for 1.5 h. The solution was diluted with 8% sodium bicarbonate solution (ca 50 ml) and the mixture extracted with ethyl acetate (3×20 ml). The extracts were dried (Na2SO4), reduced to dryness under vacuo and the residue chromatographed on silica (A). The required fractions were collected and reduced to dryness. The residue (71 mg) was dissolved in a minimum quantity of absolute ethanol and a solution of maleic acid (47 mg) in ethanol (2 ml) added. The mixture was reduced to dryness and the foam obtained stirred with dry diethyl ether (ca 5 ml). The resulting solid was collected and dried to give the title compound as a powder (78 mg), m.p. 100°-105°.

Provenance & Evidence