N,N’-二硫代二吗啉的无水制备工艺研究

Synthesis and purification of 4,4'-dithiodimorpholine( DTDM)

以吗啉和一氯化硫为原料,以固体氢氧化钠为缚酸剂合成了N,N’-二硫代二吗啉（DTDM）,考察了反应条件和重结晶条件对产物收率的影响。结果表明,较佳的合成工艺条件为：n（吗啉）∶n（S2Cl2）∶n（NaOH）=2∶1∶2,反应温度30～40℃,反应时间8 h,粗产品收率可达93%;较佳的重结晶工艺条件为：溶剂乙酸乙酯,m（溶剂）∶m（产品）=4∶1,结晶温度0～5℃,重结晶收率可达93%,DTDM总收率可达86%以上,采用FTIR与1H NMR对产物结构进行了表征。

4,4＇-Dimorpholine disulfide（ DTDM） was synthesized via addition reaction with morpholine and disulfur dichloride as starting materials and NaOH as bound acid agent. The effects of reaction conditions and purification conditions on product yield were examined. The results showed that the optimum reaction conditions were： n（ morpholine） ∶ n（ S2Cl2） ∶ n（ NaOH） =2∶ 1∶ 2,reaction temperature was 30 ～40 ℃,reaction time was 8 h,the coarse product yield can be achieved 93%; Conditions of recrystallization were： solvent was ethyl acetate,the quality of the solvent and solute ratio were 4 ∶ 1,crystallization temperature was 0 ～ 5 ℃,recrystallization yield can be achieved 93%,the yield of DTDM could reach86%. The structure of the product was characterized by FTIR and1H NMR.