Sodium Carbonate → HCID 13502279, compound

Participants

Reaction Steps

2.96 g of 3-chloro-4-(3,5-dichloro-4-methylphenyl)-4-oxobutyric acid were added to 300 ml of a 10% w/v aqueous solution of sodium carbonate, and then the resulting mixture was stirred at room temperature for 3 hours. The reaction mixture was periodically checked by thin layer chromatography and, when the spot due to the starting material had disappeared, the mixture was poured into a mixture of 500 g of crushed ice and 50 ml of concentrated hydrochloric acid. It was then extracted with diethyl ether. The ethereal extract was dried over anhydrous sodium sulfate and the solvent was then distilled off. There were obtained 2.65 g (yield 96%) of the title compound in an impure form. To this material was added a small amount of benzene, and then hexane, yielding 1.28 g (yield 46%) of the title compound in the form of pure crystals, melting at 114.5°-117.5° C.

Provenance & Evidence