1,3,2-二氧硫杂环己烷-2,2-二氧化物的合成工艺优化

Optimization of the Synthesis of 1,3,2-Dioxathiane, 2,2-dioxide

摘要:

以1,3-丙二醇和二氯亚砜为原料、高碘酸钾为氧化剂，在催化剂三氯化钌催化下合成1,3,2-二氧硫杂环己烷-2,2-二氧化物。用红外吸收光谱和核磁共振氢谱对1,3,2-二氧硫杂环己烷-2,2-二氧化物的结构进行了表征。对反应温度、反应时间、原料摩尔比、催化剂用量、氧化剂种类和氧化剂用量等工艺条件进行了优化。得到较优的操作条件为：反应温度为40 ℃，反应时间为60 min, 1,3-丙二醇 60 mmol, 原料摩尔比n(二氯亚砜):n(1,3-丙二醇)=1.2:1, 催化剂用量为1,3-丙二醇质量的0.15%，氧化剂加入量为m(高碘酸钾):m(1,3-丙二醇)=0.3:1条件下1,3,2-二氧硫杂环己烷-2,2-二氧化物的收率为92.75%。

Abstract:

The synthesis of 1,3,2-Dioxathiane 2,2-dioxide was accomplished by 1, 3-propanediol and thionyl chloride as raw materials, potassium periodate as oxidant，using ruthenium(III) chloride as catalyst. The product was characterized by IR and HNMR spectra. The effects of reaction temperature, reaction time, molar ratio of raw material, oxidant species, the amount of catalyst and oxidant on the yield of target product were investigated. The optimal condition was determined as follows: at 40 oC for 60 min, 1,3-propanediol 60 mmol, n(thionyl chloride):n(1,3-propanediol)=1.2:1, m(catalyst):m(1,3-propanediol)=0.0015, m(potassium periodate):m(1,3-propanediol)=0.3:1. The yield of the product could reach 92.75%.