Hydrogen chloride-ethyl acetate → HCID 68434236, compound

Participants

Reaction Steps

tert-Butyl (3S,5R)-3-[({2-tert-butyl-4-[(3-methoxypropyl)amino]pyrimidin-5-yl}carbonyl)(2-methylpropyl)amino]-5-(cyclopropylcarbonyl)piperidine-1-carboxylate (95 mg) was dissolved in ethyl acetate (3.2 ml), 4 M hydrogen chloride-ethyl acetate solution (0.8 ml) was added, and the mixture was stirred at room temperature for 16 hr. The solvent was evaporated under reduced pressure. The residue was subjected to reversed-phase preparative HPLC, and fractions eluted with water-acetonitrile (9:1) to acetonitrile were collected. The mixture was basified (pH 10) with saturated aqueous potassium carbonate solution, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was dissolved in ethyl acetate (5 ml), 4 M hydrogen chloride-ethyl acetate solution (75 μl) was added and the mixture was stirred for 1 min and concentrated under reduced pressure to give the object compound (48 mg).

Provenance & Evidence