Boric Acid → HCID 66673645, compound

Participants

Reaction Conditions

Reaction Steps

34.8 g of crude methyl 3-(3,5-dibenzyloxy-phenyl)-2-(4-benzyloxyphenyl)-3-oxopropionate prepared according to Example 2 (0.0608 mol) and 7.51 g of boric acid (0.121 mol) are introduced into a 250 ml round-bottomed flask. The medium is brought to 100° C. for 1 h, 120° C. for 1 h, 140° C. for 1 h and then 150-55° C. for 5 h while distilling off light products. The mixture is cooled to 60° C. and an aqueous solution of 8.5 g of sodium hydroxide pellets dissolved in 175 ml of water is added. The mixture is then brought to reflux for 3 h and brought back to 60° C., 250 ml of toluene are added, separation by settling is carried out, the organic phase is recovered and washed with 75 ml of water and then the toluene phase is concentrated on a rotary evaporator. 19.4 g of crude 1-(3,5-dibenzyloxyphenyl)-2-(4-benzyloxyphenyl)ethanone are recovered.

Provenance & Evidence