KF/Al_2O_3催化合成3-(4-苯基-1,3-二硫戊环-2-亚甲基)-2,4-戊二酮

Synthesis of α-oxo Ketene Dithioacetal with KF/Al_2O_3 as Catalyst

使用KF/Al2O3催化剂对3-(4-苯基-1,3-二硫戊环-2-亚甲基)-2,4-戊二酮进行催化合成,并确定最佳反应条件.制备KF/Al2O3催化剂,用该催化剂对乙酰基丙酮与CS2和1,2-二溴苯乙烷的反应进行催化合成制得产物,最后由红外光谱及熔点测定对产物进行表征确定.经测定,目标产物符合3-(4-苯基-1,3-二硫戊环-2-亚甲基)-2,4-戊二酮的结构特征.并确定当乙酰丙酮、CS2与1,2-二溴苯乙烷使用量为0.1mol、0.12mol、0.1mol时,最佳反应条件为催化剂使用量0.1mol,反应温度20℃,反应时间6h.在最佳反应条件下,产品收率为58.8%.KF/Al2O3催化剂可实现对3-(4-苯基-1,3-二硫戊环-2-亚甲基)-2,4-戊二酮的催化合成,且该催化反应具有产品收率高,反应时间短,反应对环境污染小等诸多优点.

Synthesis of α-oxo ketene dithioacetal with KF/Al2O3,and the optimum condition are obtained.The catalyst of KF/Al2O3 is made by ourselves and the production is synthesized from acetylaeetone with CS2 and 1-（1,2-dibromoethyl）benzene formaldehyde with catalyst,the production is defined by IR and m.p..α-oxo ketene dithioacetal is synthesized.When CH8O2、CS2 and BrCH2CH2BrPh is 0.1 mol,0.12 mol,0.1 mol respectively,the best reaction condition is that the catalyst is 0.1 mol,the reaction temperature is 20 ℃,the reaction time is 6 h, and the yield of final compound is 58.8%. The cata-lyst of KF/Al2O3 could synthesized α-oxo ketene dithioacetal. The react tion time is declined, the reaction condition is easily controlled, and the vlronment. yield is quite improved, the reac reaction is also friendly to the en