4,4′-双(氯甲基)联苯的合成研究

SYNTHESIS OF 4,4'-BIS(CHLOROMETHYL)DIPHENYL

以石油醚为溶剂,无水氯化锌为催化剂,以多聚甲醛、联苯和氯化氢气体为原料,在相转移催化剂存在下进行氯甲基化反应合成了4,4′-双(氯甲基)联苯。最佳反应条件为:n(联苯)∶n(无水氯化锌)∶n(多聚甲醛)∶n(四丁基溴化铵)=1∶1∶2.5∶0.0035,反应温度30℃,反应时间为24 h,收率达82%,纯度为97%。

4,4′-Bis（chloromethyl） diphenyl was synthesized using petroleum ether as solvent, anhy-drous zinc chloride as catalyst, and paraformaldehyde, biphenyl and hydrogen chloride as raw materals via chloromethylation in the presence of a phase-transfer catalyst. The optimal synthetic conditions were found as follows： n （biphenyl）/n （ zinc chloride）/n （paraformaldedyde）/n （tetrabutylammonium bromide） =1 ： 1 ： 2.5 ：0. 003 5, reaction temperature 30℃, reaction time 24 h. Under these conditions the yield of BCMB was 82%, and concentration of BCMB was 97% （HPLC）.