Hydrochloric Acid → HCID 70242089, compound

Participants

Reaction Steps

To a solution of the compound of Example 104 (0.85 g) in dioxan (20 ml) and methanol (10 ml) was added an aqueous solution of sodium hydroxide (2N, 5 ml). After 16 hours, the pH of the reaction was adjusted to pH5 using 1N aqueous hydrochloric acid solution and the solvent removed under reduced pressure. The crude product was purified on silica gel, eluting with a solvent gradient of 90:10:2 to 80:20:3 dichloromethane: methanol:ammonia solution. The fractions containing the product were pooled and the solvent removed under reduced pressure. The residue was taken up in a mixture of water and 1 drop of aqueous ammonium hydroxide solution and freeze-dried to give the title compound (0.65 g, 65%).

Provenance & Evidence