反应 #1256733

反应方程式

sodium hydroxide

hexylene glycol

hydrogen peroxide

sulfuric acid

→

Hexylene glycol hydroperoxide

反应条件

后处理

1. 1
   其他After separation the underlayer
2. 2
   workup.ADDITIONThe remaining crude hexylene glycol hydroperoxide was converted to sodium salt by the addition of 160 g of a 25% NaOH solution
3. 3
   萃取Subsequently, the sodium salt was extracted 3 times with ethyl ether in order

实验过程

Hexylene glycol hydroperoxide was prepared by reaction of 118.1 g (1.0 mol) hexylene glycol and 145.7 gr (3 mol) hydrogen peroxide in the presence of sulfuric acid at a temperature of 30° C. for 1 hour. The reaction mixture was cooled down to 20° C. and neutralized with sodium hydroxide until pH=6.8. After separation the underlayer was drained. The remaining crude hexylene glycol hydroperoxide was converted to sodium salt by the addition of 160 g of a 25% NaOH solution. Subsequently, the sodium salt was extracted 3 times with ethyl ether in order to lower the dialkyl peroxide content (di(3-hydroxy-1,1-dimethylbutyl)peroxide). The remaining sodium salt of hexylene glycol hydroperoxide was acidified with H2SO4 25% until pH 3. Hexylene glycol hydroperoxide was isolated from the solution with ethyl ether. After evaporation of the ethyl ether the resulting product was analysed and found to contain 92% hexylene glycol hydroperoxide.

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