HCID 14392657, compound → HCID 14392652, compound

Participants

Reaction Steps

A mixture of the product of stage (i) (0.8 g) in ethanolic hydrogen chloride (80 ml) was hydrogenated over pre-reduced 10% palladium on carbon (50% paste with water, 0.8 g) until uptake ceased. The catalyst was filtered off, washed with hot ethanol (50 ml) and the filtrate evaporated in vacuo to give crude material (0.15 g). The catalyst residues were then warmed (70°) with 2N hydrochloric acid (200 ml), filtered and the filtrate evaporated to dryness in vacuo (azeotroped with toluene). The residue was combined with the crude product obtained above and purified by flash chromatography (silica 9385, 100 g) eluting with CH2Cl2 /EtOH/NH3 (50:8:1) to give the title compound as a solid (0.2 g) m.p. >95° (foams),

Provenance & Evidence