Boric Acid → HCID 66674733, compound

Participants

Reaction Conditions

Reaction Steps

90.9 g of crude methyl 3-(3,5-dimethoxyphenyl)-2-(3,4-dimethoxyphenyl)-3-oxopropionate prepared according to Example 3 and 30 g of boric acid are introduced into a 250 ml three-necked round-bottomed flask. The mixture is heated with stirring at 100° C. for 1 h, 120° C. for 1 140° C. for 1 h and then 160° C. for 4 h while distilling off light products. The mixture is cooled to approximately 60° C., 226 g of a 15% sodium hydroxide solution are added dropwise and the mixture is maintained at reflux for 2 h with stirring. The reaction medium is extracted at ambient temperature with 350 ml of toluene, which is washed with 100 ml of water. The organic phase is concentrated to recover 51.70 g of 1-(3,5-dimethoxyphenyl)-2-(3,4-dimethoxyphenyl)ethanone in the form of an oil with a dark brown colour.

Provenance & Evidence