Methanol → HCID 68281549, compound

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Reaction Steps

Pd/C (10%, 50% wet) (2 g; 50% by mass) is added to a solution of compound (16) (4 g; 70% by mass; 6.8 mmol, 1.0 eq) in a methanol/1 M aqueous HCl solution mixture (120 ml/40 ml). The suspension is stirred for 4 days under hydrogen atmosphere and then filtered using a Buchner funnel. The filtrate is evaporated under reduced pressure. The oil obtained is taken up in 1 M aqueous sodium hydroxide solution (160 ml) and washed with ethyl acetate (2×80 ml). The aqueous phase is neutralized by adding solid NaH2PO4 and then filtered using a Buchner funnel. The solid obtained is washed thoroughly with water and then dried under strong vacuum to lead to compound 3 (0.5 g; 35%) obtained as a beige solid.

Provenance & Evidence