Hydrochloric Acid → HCID 86735631, compound

Participants

Reaction Conditions

Reaction Steps

12 Mmol (5.1 g) of 5-chloro-4'-trifluoromethylvalerophenone O-(2-aminoethyl) oxime maleate (1:1) (melting point 121.5°-122.5° C) were added to a solution of 240 mgat. (5.5 g) of sodium in 100 ml of absolute ethanol. The mixture was heated at 70° C for 8 hours followed by neutralization at 0° C with alcoholic hydrochloric acid and the sodium chloride was filtered off. The alcohol was distilled off in vacuo and the residue was dissolved in water. 5 Ml of 50% sodium hydroxide solution were added to this solution and three extractions with 40 ml of ether were then carried out. The ether extract was washed with 5% sodium bicarbonate solution (1x) and with water (1x), followed by drying on sodium sulphate. The ether was distilled off in vacuo and the residue was dissolved in absolute ethanol. The solution was acidified with an equimolar quantity of fumaric acid. The title compound crystallized from the solution. Melting point 105°-105.5° C.

Provenance & Evidence