Pyridine → 1197-50-8

Participants

Reaction Steps

Phenylpropionaldehyde (3.35 g, 3.3 ml, 25 mmol) was dissolved in EtOH (90 ml) and mixed successively with hydroxylamine hydrochloride (2.6 g, 37.5 mmol) and abs. pyridine (2.42 ml, 30 mmol) while stirring. After stirring for 4 h, the solvent was removed under vacuum, the residue taken up in toluene (1×50 ml) and the solvent removed again under vacuum. The oily residue was stirred with EtOAc (50 ml) and water (30 ml) for 15 min. Subsequently, the phases were separated. The organic phase was washed with water (2×20 ml), dried and concentrated. The oil obtained (4.71 g) was highly contaminated and crystallised only in part. The oil was dissolved in n-hexane (20 ml) and stored for 18 h at 5° C. The precipitated plates were removed by suction-filtration. Compound Z was obtained as a white solid in a yield of 24% (892 mg) having a melting point of 85-93° C.

Provenance & Evidence