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
20.0 g (0.104 mol) of 4-cyclohexylresorcinol are dissolved in 40 ml of ten percent strength sodium hydroxide solution and are hydrogenated in the presence of 5 g of Raney nickel in an autoclave at 90° under 20 bar for 5 hours. The reaction mixture is rinsed out of the autoclave with alcohol. After removal of the catalyst, 100 ml of 90 percent strength acetic acid are slowly added to the solution. After addition of water, the reaction product crystallises out. It is dried in vacuo over NaOH. 12.9 g of 1,3-dioxo-6-cyclohexyl-cyclohexane of melting point 137°-140° C. are obtained. After recrystallisation from ethyl acetate, the product has a melting point of 142°-144° C. (literature). Yield: 11.1 g (=55%).
WORKUP
后处理
- washThe reaction mixture is rinsed out of the autoclave with alcohol
- customAfter removal of the catalyst, 100 ml of 90 percent strength acetic acid
- additionare slowly added to the solution
- additionAfter addition of water
- customthe reaction product crystallises out
- dry with materialIt is dried in vacuo over NaOH