3,5-二羟基甲苯的合成研究

Study on synthesis of orcinol

采用廉价的3-甲基-4-氯苯酚为原料,通过高温脱氯水解一步反应制得中间体3,5-二羟基甲苯的酚钾盐,然后酸化处理制得标题化合物。对原料配比、溶剂种类、溶剂量、反应温度、反应时间和脱水剂等工艺条件进行了详细研究。结果表明,采用均三甲苯为溶剂,并用分水器分出反应生成的水。在164～166℃回流反应约14h,处理后可得纯度大于98%的产品,收率40%以上。该方法工艺短,收率较高,原料廉价易得,是一种有前途的方法。

For searching the new method of synthesis of orcinol, the cheap 3-methyl-4-chlorophenol was taken as starting material, and the intermediate potassium salt of 3,5-dihydroxy phenol was obtained via high-temperature de-chloro and hydrolysis reaction. After treatment by acid and work up, the title compound was obtained. The conditions of procedure, such as the ratio of raw materials, the solvents and the quantity of solvent, temperature, reaction time and de-hydrolyzing agent were investigated in detail. It has been found that using 1,3,5-trimethylbenzene as solvent, removing the water produced in reaction, refluxing at 164～166 ℃ for about 14 hrs, the title compound was afforded in 40% yield with more than 98% purity. The method is considered a good one with advantages such as short procedure, high yield, and starting material cheap and easy to get.