Sulfuric Acid → HCID 54064055, compound

Participants

Reaction Steps

3 ml of ethanol and 0.5 ml of carbon tetrachloride are added to 1.4 g of magnesium turnings. After initiation of the reaction, a mixture of 8.7 g of diethyl malonate, 6 ml of ethanol and 23 ml of toluene are added at 50° C. The mixture is warmed for 1 hour at 50°-60° C. and then cooled to -5°--10° C. A solution of 13.3 g of 2,4-dichloro-5-fluoro-3-methylbenzoyl chloride (from 2,4-dichloro-5-fluoro-3-methylbenzoic acid and thionyl chloride) in 6 ml of toluene is added dropwise at this temperature. The mixture is then allowed to come to room temperature. After standing overnight, a mixture of 24 ml of water and 4 ml of H2SO4 is added. The phases are separated, and the organic phase is washed with water, dried and concentrated. 20 ml of water and 0.1 g of p-toluenesulphonic acid are added to the oily residue. The mixture is refluxed for 4.5 hours, the phases are subsequently separated, and the organic phase is dried and concentrated in vacuo. 14.1 g of the titled compound remain as a crude oil. ##STR12##

Provenance & Evidence