Pyridinium chloride → HCID 20368375, compound

Participants

Reaction Steps

A mixture of 2.5 g. (0.0073 mole) of the product from Example 5 and 10 g. of pyridine hydrochloride was refluxed in a 220° C. oil bath for 1.5 hours. The hot reaction mixture then was poured over an ice-water mixture in a blender, and the resulting yellow crystals were collected. The crystals then were dissolved in ethyl acetate, and the ethyl acetate solution was washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The ethyl acetate solution then was filtered over silica, and the silica was washed with ethyl acetate which was added to the original ethyl acetate solution. The ethyl acetate was evaporated and the resulting residue was crystallized from methanol to give 2.1 g. (88 percent) of the title compound as yellow crystals, m.p. 187°-190° C. The product was recrystallized from methanol to give a purified product having melting point 191°-191.5° C.

Provenance & Evidence