Potassium Hydroxide → HCID 136227081, compound

Participants

Reaction Steps

The ketone of Example 30 (7.5g,0.03mole) in ethanol (18ml) was added with stirring to a solution of (85%) potassium hydroxide (20.74g, 0.3mole) in water (85ml) at 10°C, this colloidal solution was treated with solid hydroxylamine hydrochloride (8.54g,0.12 mole) and stirred overnight. The solution was acidified with 5NHCl to give a solid, which was filtered, washed with water and stirred for 45 minutes, with 5% Na2CO3 solution (30.5ml), to remove unwanted oxime stereoisomer, filtered, washed with 5% Na2CO3 solution (100ml) 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") 5.45g.

Provenance & Evidence