Hydrochloric Acid → HCID 20640389, compound

Participants

Reaction Steps

Aqueous sodium hydroxide solution (3 ml, 2N) was added to a solution of the compound from Example 37 (580 mg), in dioxan (6 ml) and methanol (3 ml) and the reaction stirred at room temperature for 3 hours. The reaction mixture was acidified to pH 5 using 2N hydrochloric acid then evaporated to dryness in vacuo. The residue was purified by column chromatography over silica gel using gradient elution (85/15/2.5-80/20/3 dichloromethane/methanol/ammonium hydroxide). This material was further purified on a polystyrene reverse phase resin using gradient elution (100/0-50/50 water/acetonitrile). The acetonitrile was evaporated in vacuo and the remaining aqueous solution was frozen and lyophilised to afford the title compound, 410 mg.

Provenance & Evidence