Acetic Acid → HCID 53668369, compound

Participants

Reaction Conditions

Reaction Steps

Into a 100 ml four-necked flask were charged 12.12 g of above-obtained 4-(4-hydroxy-3-methylbenzyl)-2,5-dimethylphenol having a purity of 90.05%,4.8 g of sodium hydroxide and 48 g of water. While stirring at 40° C., 24.35 g of 37% formaldehyde was added dropwise thereto over 1 hour, and the reaction was conducted for 2 more hours. After completion of the reaction, 10 g of 90% aqueous acetic acid solution was added for neutralization and then the mixture was cooled to 25° C. The resulting mixture was filtered and rinsed with 100 g of deionized water. The filtered product was dissolved in 200 g of ethyl acetate, 50 g of toluene was added thereto and the resulting mixture was concentrated. To the concentrated mass, 200 g of toluene was added, and the mixture was cooled to 20° C., and then filtered. The filter cake was rinsed with 200 g of toluene and dried a whole day and night under reduced pressure at 45° C. to obtain 9.20 g of 2-hydroxymethyl-4-(4-hydroxy-3-hydroxymethyl-5-methylbenzyl)-3,6-dimethylphenol.

Provenance & Evidence