Water → HCID 12765967, compound

Participants

Reaction Steps

29.7 g (0.55 mol) of sodium methylate were dissolved in 500 ml of methanol and 70.4 g (0.55 mol) of 4-chlorophenol were added to the solution, whilst stirring. After the mixture had been stirred for 10 minutes, the solvent was distilled off under reduced pressure and the residue was taken up in 100 ml of glycol. This solution was added to a solution of 135 g (0.5 mol) of 2,2-dimethyl-1-tosyloxy-butan-3-one in 200 ml of glycol. The reaction mixture was stirred for 48 hours at 100° to 120° C., and was cooled and stirred into 2,000 ml of water. The mixture was extracted with twice 250 ml of diethyl ether, and the combined organic phases were washed with three times 100 ml of water, once with 100 ml of 10% strength sodium hydroxide solution and again with 100 ml of water, dried over sodium sulphate and distilled. 62.9 g (55.7% of theory) of 1-(4-chlorophenoxy)-2,2-dimethylbutan-3-one of boiling point 135°-140° C./0.4 mm Hg were obtained. ##STR10##

Provenance & Evidence