Hydrochloric Acid → HCID 22131463, compound

Participants

Reaction Steps

A Parr® hydrogenation flask was charged with the title product of Example 2 (1.90 g, 4.61 mmol), 10% Pd/C (0.58 g), 95% ethanol (20 mL), and conc. HCl (0.96 mL, 12 mmol). The mixture was hydrogenated, under hydrogen at 276 kPa (40 psi), for 19 hours. The catalyst was removed by filtration through Celite®, and the filtrate was concentrated to provide an oily, yellow-white solid, which was 85% pure by HPLC analysis. A portion of this material was purified as its free base (i.e., the HCl salt was dissolved in methanol, treated with one molar equivalent of K2CO3 filtered and concentrated) by silica gel chromatography, eluting with 500:50:1 CH2Cl2 -methanol-NH4OH, providing the title product as a white solid which was homogenous by HPLC analysis.

Provenance & Evidence