Hydrochloric Acid → HCID 70528399, compound

Participants

Reaction Steps

163 g (2.2 mols) of formic acid ethyl ester were added dropwise to a solution of 136 g of sodium ethylate in 1,500 ml of ethanol at 0° C. 420 g (2 mols) of 2,2-dimethyl-4-(4-fluorophenoxy)-butan-3-one were then slowly stirred in at 0° C. After a reaction time of 24 hours at 0° C., the mixture was allowed to warm to room temperature and was subsequently stirred at this temperature for a further 96 hours. The reaction mixture was poured into 5,000 ml of ice-water and the organic phase was separated off by extraction with chloroform. Unreacted starting material could be isolated from this chloroform solution and could be employed again. The aqueous phase was acidified with 10% strength hydrochloric acid, while cooling, and the oil which separated out was taken up in chloroform. The chloroform phase was dried over sodium sulphate and concentrated by distilling off the solvent in vacuo. The oil which remained was distilled in vacuo. 170 g (83% of theory, relative to reacted material) of 1-hydroxy-2-(4-fluorophenoxy)-4,4-dimethyl-1-penten-3-one of boiling point 101°-102° C./0.6 mm Hg (nD20 =1.5132) were obtained. ##STR50##

Provenance & Evidence