Acetic Acid → 1,3-Benzenedimethanol, 4-hydroxy-2,5,6-trimethyl-

Participants

Reaction Conditions

Reaction Steps

Into a 2 liter four-necked flask were charged 136.19 g of 2,3,5-trimethylphenol, 48.0 g of sodium hydroxide and 480 g of water. While stirring at 40° C., 486.91 g of 37% formaldehyde was added dropwise thereto over one hour, and the reaction was conducted for 3 more hours. After completion of the reaction, 180.15 g of 90% aqueous acetic acid solution was added for neutralization, then the mixture was cooled to25° C. and filtered. The filtrate was extracted with 1000 g of ethylacetate and the ethyl acetate layer was washed with water and concentrated.To the concentrated mass, 500 g of toluene was added and the mixture was cooled to 20° C. and filtered. The filter cake thus obtained was rinsed with 400 g of toluene and dried a whole day and night at 45°C. under reduced pressure to obtain 100 g of 2,4-bis(hydroxymethyl)-3,5,6-trimethylphenol.

Provenance & Evidence