【摘要】 1,2-二硫戊烷叔胺类化合物Ⅷ的合成途径如下:溴丙烯经Prins反应得4-溴代次甲基-1,3-二氧六环己烷Ⅹ,再与仲胺缩合得相应的取代叔胺二氧六环己烷Ⅺ,后者经水解得2,4-丁二醇胺Ⅻ。将Ⅺ或Ⅻ与硫脲及氢碘酸长时间反应,水解后用碘氧化,即得产物Ⅷ。其中化合物Ⅷ_a和ⅩⅣ_e对小白鼠急性电离辐射损伤有弱防护效果。更多还原

【Abstract】 Some tertiary amino derivatives of 1,2-dithiolane (Ⅷ) were synthesized as follows: Allylbromide was reacted with conc. sulfuric acid and paraformaldehyde to give 4-bromomethyl-1,3-dioxane(Ⅹ),which was reacted with excess secondary amine to yield the corresponding tertiary amino derivatives of 1,3-dioxane (Ⅺ). (Ⅺ) was hydrolyzed by hydrochloric acid in methanol to give (Ⅻ). When (Ⅺ) or (Ⅻ) was treated With conc. hydroiodic acid in the presence of thiourea, the dithiol intermediate formed was then oxidized by iodine to yield the final product (Ⅷ).When (Ⅻ) was treated with hydrobromic acid instead of hydroiodic acid in the presence of thiourea, only the monothiol derivative of the corresponding amino alcohol (ⅩⅣ) was obtained, the exact position of the thiol or the hydroxy group in the molecule remained unknown. An attempt to prepare the primary aminoderivative of 1,2-dithiolane through the reaction of (ⅩⅧ) with thiourea or potassium thioacetate, followed by hydrolysis and oxidation of the intermediate failed. In these cases only the monosubstitution product (ⅩⅨ) or (ⅩⅩ) was obtained.Compd (ⅩⅪ) wasobtained by the treatment of (Ⅻ) with thionylchloride, it failed to react with sodium polysulfide to yield the corresponding amino dithiolane derivative.Compds Ⅷ_a and ⅩⅣ_e exhibited weak protective activity against ionization radiation in mice.更多还原