8-硫-1,6-二氮双环[4.3.0]壬烷-7,9-二酮的合成及单晶结构

Synthesis and structure characterization of 8-thia-1, 6-diazabicyclo[4.3.0] nonane-7, 9-dione

摘要:

以二硫化碳、甲醇、氢氧化钾为起始原料，经3步反应生成5-甲氧基-1,3,4-噻二唑-2(3H)-酮，再与1,4-二溴丁烷进行取代，然后脱甲基，最后发生亲核取代得8-硫-1,6-二氮双环[4.3.0]壬烷-7,9-二酮。利用1HNMR、13CNMR等对产物结构进行了表征，通过X-射线衍射测定了目标产物的单晶结构，该化合物属于三斜晶系，P1空间群，晶胞参数a =7.8400(16) ?，b =10.464(2) ?，c =10.514(2) ?，α=63.84(3)?，β=79.62(3)?γ=89.42(3)?，V =759.2(3) ?，Z =4，wR(F2) =0.125，μ=0.37mm-1。

Abstract:

3,4-thiadiazol-2-one with 1,4-dibromobutane which was then demethylated then intramolecular alkylated. 5-Methoxy-3H-1, 3, 4-thiadiazol-2-one was synthesized by three steps with CS2, CH3OH and KOH as raw materials.The structures of the compounds were characterized by 1H NMR and 13CNMR spectra. The crystal structure of target compound was determined by X-ray single crystal diffraction. Target compound belongs to the triclinic, space group P1, with a =7.8400(16) ? b =10.464(2) ? c =10.514(2) ? α=63.84(3)? β=79.62(3)? γ=89.42(3)? V =759.2(3) ?, Z =4, wR(F2) =0.125, μ=0.37mm-1。