反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customare reacted in a stirred autoclave at 180° C. under autogenous pressure of 20-30 bar for 10 h
- temperatureAfter the autoclave has cooled
- distillationWorkup of the mixture by distillation