光学活性拆分剂脱氢枞胺的制备性纯化及其表征

Purification and Characterization of Optically Active Resolving Reagent Dehydroabietylamine

采用松香胺与对甲基苯磺酸成盐法,对光学活性拆分剂脱氢枞胺的纯化工艺进行了改进.通过对甲基苯磺酸与工业产品松香胺D在乙醇中形成脱氢枞胺、双脱氢枞胺、四脱氢枞胺的对甲基苯磺酸盐,经重结晶分离得到光学纯度的脱氢枞胺的对甲基苯磺酸盐,再利用碱游离得到光学纯度的脱氢枞胺.最后通过红外光谱、核磁共振光谱及高效液相色谱等对其进行表征.

The purification process of dehydroabietylamine was improved, whereby the industrial rosin amine D was reacted with p -toluenesulfonic acid in ethanol to get a mixture of dehydro-abietylamine p -toluenesulfonate, didehydroabietylamine p -toluenesulfonate, and tetradehydro-abietylamine p -toluenesulfonate. The mixture was separated by recrystallization to get pure dehydroabietylamine p -toluenesulfonate. Then pure dehydroabietylamine was obtained by reacting dehydroabietylamine p -toluenesulfonate with sodium hydroxide. The structure of dehydro-abietylamine was characterized by IR ()~1HNMR and HPLC.