以α D 葡萄糖为原料经过乙酰化、溴化、硫氰酸化三步反应合成了 2, 3, 4, 6 四 O 乙酰基 β D 吡喃葡萄糖基异硫氰酸酯。用NMR对其进行了表征。考察了相转移催化剂种类及用量、反应时间、溶剂对反应的影响。得出最佳反应条件为:以苯做...以α D 葡萄糖为原料经过乙酰化、溴化、硫氰酸化三步反应合成了 2, 3, 4, 6 四 O 乙酰基 β D 吡喃葡萄糖基异硫氰酸酯。用NMR对其进行了表征。考察了相转移催化剂种类及用量、反应时间、溶剂对反应的影响。得出最佳反应条件为:以苯做溶剂,物料摩尔比为n(2, 3, 4, 6 四 O 乙酰基 α D 吡喃溴代葡萄糖)∶n(硫氰酸钾 )∶n(三乙基苄基氯化铵) =1∶2∶1,反应时间为 14h。把它用作柱前衍生试剂拆分异构体,测定了对映体过量 (ee)值,均得到了满意的结果。展开更多
N-substituted phosphoramidic chloride was obtained from the reaction of amines with POCl3,then hydrazinolyzation gave N-substituted phosphoramidohydrazide（2a-2g）.Refluxing of 2 with glucosyl isothiocyanate（1）in CH...N-substituted phosphoramidic chloride was obtained from the reaction of amines with POCl3,then hydrazinolyzation gave N-substituted phosphoramidohydrazide（2a-2g）.Refluxing of 2 with glucosyl isothiocyanate（1）in CHCl3 gave corresponding N,N′-substituted-N″-（2,3,4,6-tetra-O-acetylglucosylthioureylene）phosphoric triamides（3a-3g）,and deacetylation in MeOH/NaOMe gave N,N’-substituted-N″-glucosy1 thioureylene phosphoric triamides（4a-4g）.Their structures were confirmed by IR,1H NNR,31P NMR,MS and elemental analysis.展开更多
文摘N-substituted phosphoramidic chloride was obtained from the reaction of amines with POCl3,then hydrazinolyzation gave N-substituted phosphoramidohydrazide（2a-2g）.Refluxing of 2 with glucosyl isothiocyanate（1）in CHCl3 gave corresponding N,N′-substituted-N″-（2,3,4,6-tetra-O-acetylglucosylthioureylene）phosphoric triamides（3a-3g）,and deacetylation in MeOH/NaOMe gave N,N’-substituted-N″-glucosy1 thioureylene phosphoric triamides（4a-4g）.Their structures were confirmed by IR,1H NNR,31P NMR,MS and elemental analysis.
