Hydrochloric Acid → HCID 136227081, compound

Participants

Reaction Steps

The ketone of Example 4 (7.5 g, 0.03 mole) in ethanol (18 ml.) was added with stirring to a solution of (85%) potassium hydroxide (20.74 g, 0.3 mole) in water (85 ml) at 10° C., this colloidal solution was treated with solid hydroxylamine hydrochloride (8.54 g, 0.12 mole) and stirred overnight. The solution was acidified with 5N HCl to give a solid, which was filtered, washed with water and stirred for 45 minutes, then treated with 5% Na2CO3 solution (30.5 ml), to remove unwanted oxime stereoisomer, filtered, washed with 5% Na2CO3 solution (100 ml) and then with water until free of alkali. The dried solid had m.p. 175°-177° C. Recrystallisation from 54% benzene-light petroleum (b.p. 60°-80° C.) mixture gave the oxime, m.p. 178° C. ("bonded isomer") 5.45 g.

Provenance & Evidence