HRID361978

反应详情

EQUATION

反应方程式

HRID 361978 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Into a 100 ml four-necked flask were charged 7.69 g of the above-obtained 4-(2-hydroxy-4,5-dimethylbenzyl)-2,5-dimethylphenol having purity of 90.85%, 2.88 g of sodium hydroxide and 28.8 g of water and they were dissolved. While keeping the temperature at 40° C., 14.61 g of 37% formaldehyde was added dropwise thereto over one hour, and the mixture wasstirred for one more hour. After completion of the reaction, 6 g of 90% aqueous acetic acid solution was added for neutralization and the mixture was cooled to 25 ° C. Thereafter, 100 g of ethyl acetate and 20 g of toluene were added thereto, followed by a phase separation. The solution thus obtained was concentrated to obtain 9.20 g of 2-hydroxymethyl-4-(2-hydroxy-3-hydroxymethyl-4,5-dimethylbenzyl)-3,6-dimethylphenol

WORKUP

后处理

  1. dissolutionwere dissolved
  2. customat 40° C.
  3. additionwas added for neutralization
  4. customfollowed by a phase separation
  5. customThe solution thus obtained
  6. concentrationwas concentrated