HRID1464477

反应详情

EQUATION

反应方程式

HRID 1464477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

125 g (1 mol) of 80% strength aqueous 2,2-dimethyl-3-hydroxypropanal (crude mixture from the synthesis, reduced to a water content of 20%. by distillation), 109 g (0.9 mol) of 2,6-dimethylphenol, 12 g (0.11 mol) of 40% strength aqueous dimethylamine and 700 g of methanol are reacted in a stirred autoclave at 180° C. under autogenous pressure of 20-30 bar for 10 h. After the autoclave has cooled and the pressure has been released, 19 g of Raney Ni (0.02 parts based on complete mixture) are added to the reaction mixture and hydrogenation is carried out at 80° C. under 80 bar of hydrogen for 5 h. Workup of the mixture by distillation yields 174 g (92%) of 3-(3,5-dimethyl-4-hydroxyphenyl)-2,2-dimethylpropanol (boiling point 172°-174° C.; melting point 133°-134° C.).

WORKUP

后处理

  1. customare reacted in a stirred autoclave at 180° C. under autogenous pressure of 20-30 bar for 10 h
  2. temperatureAfter the autoclave has cooled
  3. distillationWorkup of the mixture by distillation