A clean and safe synthesis method of 5-(4'-methylbiphenyl-2-yl)-1H-tetrazole was found:under hydrothermal conditions,1.2 equiv.of 4'-methylbiphenyl-2-carbonitrile react with 1 equiv.of sodium azide in a mixed solvent of propane-1,2-diol/H2O,with 1.5 equiv.of ammonium chloride and 0.2 equiv.of ammonium fluoride as catalyst.After simple post-processing,the yield can be improved to 95%,and the purity of the product is 99%without further recrystallization.
核磁共振(nuclear magnetic resonance,NMR)是以原子核自旋的共振跃迁为探测对象的谱学方法.当自旋量子数不为零的原子核处于外磁场中时,会引起能级的Zeeman分裂.若再施加能量等于Zeeman能级差的射频场,则会诱发原子核自旋的共振跃迁,这种现象即为核磁共振.核自旋的共振频率与原子的类型有关,且受原子所处化学和物理环境的影响.此外,NMR能量较低,不会影响探测对象(常为分子)的状态.因此,NMR能够在无损条件下提供多种具有原子和分子分辨的物质组成、结构、形态、动态变化等丰富信息.
Crab paste is a traditional and popular food for people in the coastal area of China.Visual inspection is currently the only method of quality assessment.We developed a new analytical method of a comprehensive survey of nutrients and quality assessment for crab paste based on a combination of 1 H NMR spectroscopy with multivariate data analysis.The aqueous extract of crab paste was dominated by amino acids,sugars,carboxylic acids,nucleotides and amines(including 19 first-time-reported compounds such as choline,uracil and guanosine).Two grades of crab paste had significant compositional differences in terms of amino acids,lactate,N-acetylglutamate,choline,dimethylamine,uridine,1-methylnicotinamide and 2-pyridienmethanol.These results provided important information on the grade-dependence of crab-paste composition,and demonstrated that NMR-MDA was effective not only for the comprehensive survey of nutrients,but also for quality assessment of crab paste.
