Acetic Acid → HCID 54251996, compound

Participants

Reaction Conditions

Reaction Steps

Into a 500 ml four-necked flask were charged 40.45 g of above-obtained 2,4-bis(4-hydroxy-2,5-dimethylbenzyl)-3,5,6-trimethylphenol having a purity of 99.38%, 14.4 g of sodium hydroxide, 144 g of water and 14.4 g oftetrahydrofuran and they were completely dissolved. While stirring at 40° C., 48.69 g of 37% formaldehyde was added dropwise thereto over1 hour, and the reaction was conducted for 3 more hours. After completion of the reaction, 18.02 g of 90% aqueous acetic acid solution was added forneutralization and then the mixture was cooled to 25° C. The resulting mixture was filtered and the filtered product was dissolved in amixed solvent consisting of 100 g of ethyl acetate and 14.40 g of tetrahydrofurane. The resulting solution was washed with water and the oilphase was concentrated. To the concentrated product, 100 g of toluene was added, and the mixture was cooled to 20° C., and then filtered. Thefilter cake was rinsed with 100 g of toluene and dried a whole day and night under reduced pressure at 45° C. to obtain 36.8 g of 2,4-bis(4-hydroxy-3-hydroxymethyl-2,5-dimethylbenzyl)-3,5,6-trimethylphenol.

Provenance & Evidence