Methane → HCID 20041374, compound

Participants

Reaction Steps

A solution of the product of Stage (i) (20.5 g) in ethanol (150 ml) containing 2N hydrochloric acid (150 ml) was stirred in the presence of 10% palladised charcoal (2.0 g) under an atmosphere of hydrogen, until uptake ceased. The suspension was filtered through a pad of `hyflo`, the pad was washed with 50% aqueous ethanol (200 ml) and the combined filtrates evaporated under reduced pressure. Crystallisation of the residue from methanol-isopropyl acetate [1:1] (300 ml) gave the title compound as a powder (23.7 g), m.p.>300°.

Provenance & Evidence