本芴醇的合成工艺改进

Improvement of the Synthesis Process of Benfluorenol

以芴(2)为原料,经三氯异腈尿酸氯化得2,7-二氯芴(3),与氯乙酰氯发生酰化反应生成2,7-二氯芴-4-氯乙酮(4),再将还原、环合、胺化“一锅法”合成得到α-(二正丁胺甲基)-2,7-二氯-4-芴甲醇(5),最后与对氯苯甲醛缩合得到本芴醇(1),总收率36%,纯度99.4%。新工艺中的氯化采用三氯异腈尿酸为氯化剂,反应选择性与安全性提高;还原、环合与胺化运用“一锅法”完成,反应温度降低,反应周期缩短,生产效率提高(从60%提高到80%),适合放大生产。

Using fluorene(2)as the starting material,it was chlorinated by trichloroisocyanuric acid to obtain 2,7-dichlorofluorene(3),which was acylated with chloroacetyl chloride to produce 2,7-dichlorofluorene-4-chloroethyl ketone(4).Then,α-(di-n-butylaminomethyl)-2,7-dichloro-4-fluorenylmethanol(5)was obtained via reduction,cyclization and amination by one-pot method.Finally,5 was condensed with p-chlorobenzaldehyde to obtain benfluorenol(1),with an overall yield of 36%and a purity of 99.4%.The improved process used trichloroisocyanuric acid as the chlorinating agent,which improved the selectivity and safety of the reaction.The reduction,cyclization and amination were completed by onepot method,which reduced the reaction temperature,shortened the reaction cycle,improved production efficiency,and increased the yield from 60%to 80%.The improved process was simple to operate,low in production cost and suitable for industrial production.