4,4′-二硫代二吗啉的合成及重结晶工艺研究

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

以吗啉和一氯化硫为原料,在无水体系中,以过量的吗啉做缚酸剂合成了4,4′-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)=4∶1,反应温度30~40℃,反应时间6h,粗产品收率可达96%;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】93%,DTDM总收率】90%,采用FT-IR与1 H 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 morpholine as bound acid agent in without water system.The effects of reaction conditions and purification conditions on product yield were examined.The results showed that the addition reaction conditions are:n(morpholine)∶n(S2Cl2)=4∶1,reaction temperature is 30~40℃,reaction time is 6h.The yield of coarse product can be achieved 96%.Better conditions of recrystallization are:using ethyl acetate as solvent,the mass ratio of the solvent and solute ratio is 4∶1,crystallization temperature is 0~5℃.The recrystallization yield can reach 93.0%,the yield of DTDM can reach 90.0%.The structure of the product was characterized by FT-IR and1 H NMR.