反应详情

温度

20 °C

Into a 1 liter of four-necked flask were charged 1.90 g of para-toluene sulfonic acid, 24.43 g of 3,4-xylenol and 48.87 g of toluene. Further, keeping the temperature at 30° C., 7.61 g of 4-hydroxymethyl-2,5-dimethylphenol was added in ten portions over 1 hour. The mixture was stirred at the same temperature for 2 more hours. After completion of the reaction, 50 g of toluene and 50 g of ethyl acetate was added. Thereafter, 50 g of deionized water was added and the resulting mixture was stirred and a phase separation was carried out. Then, metal content was removed by adding 50 g of 1% aqueous oxalic acid solution, followed by stirring the mixture and by carrying out a phase separation. Thereafter, washing with 50 g of deionized water was repeated four times, and the oil phase was concentrated. To the concentrated mass, 100 g of toluene was added and the resulting solution was cooled to 20° C. and filtered. The filter cake was rinsed with 200 g of toluene and dissolved in 50 g of ethyl acetate. After adding 200 g of toluene thereto,the resulting mixture was concentrated. To the concentrated mass, 100 g of toluene was added and the resulting mass was cooled to 20° C. and filtered. The filter cake was rinsed with 100 g of toluene and dried a whole day and night under reduced pressure at 45 ° C. to obtain 8.82 g of 4-(2-hydroxy-4,5-dimethylbenzyl)-2,5-dimethylphenol.

1. customat 30° C.
2. additionwas added
3. stirringthe resulting mixture was stirred
4. customa phase separation
5. customThen, metal content was removed
6. additionby adding 50 g of 1% aqueous oxalic acid solution
7. stirringby stirring the mixture
8. customa phase separation
9. washThereafter, washing with 50 g of deionized water
10. concentrationthe oil phase was concentrated
11. additionTo the concentrated mass, 100 g of toluene was added
12. filtrationfiltered
13. washThe filter cake was rinsed with 200 g of toluene
14. dissolutiondissolved in 50 g of ethyl acetate
15. additionAfter adding 200 g of toluene
16. customthereto,the resulting mixture
17. concentrationwas concentrated
18. additionTo the concentrated mass, 100 g of toluene was added
19. temperaturethe resulting mass was cooled to 20° C.
20. filtrationfiltered
21. washThe filter cake was rinsed with 100 g of toluene
22. customdried a whole day and night under reduced pressure at 45 ° C.