报道了9-[(4氟-)-3羟-基甲基丁基]鸟嘌呤(FHBG,Ⅱ)的改进合成方法,对起始原料喷昔洛韦(Ⅲ)的氨基和一个羟基用4-甲氧基氯化三苯甲烷保护,对另一个羟基磺酯化,得到N2-(p-甲氧基苯酰基二苯基甲基)-9-[(4甲-苯磺酰)-3-p-甲氧基苯酰基二苯基...报道了9-[(4氟-)-3羟-基甲基丁基]鸟嘌呤(FHBG,Ⅱ)的改进合成方法,对起始原料喷昔洛韦(Ⅲ)的氨基和一个羟基用4-甲氧基氯化三苯甲烷保护,对另一个羟基磺酯化,得到N2-(p-甲氧基苯酰基二苯基甲基)-9-[(4甲-苯磺酰)-3-p-甲氧基苯酰基二苯基-甲氧基甲基丁基]鸟嘌呤(Ⅴ),收率为70.5%;再用四丁基氟化铵(TBAF)对化合物Ⅴ亲核取代4-甲苯磺酰基团,水解脱去保护基,即得FHBG。产品经1HNMR、IR、MS表征,并用HPLC分析了Ⅴ和Ⅱ,保留时间分别为5.89 m in和4.41 m in,积分计算质量分数分别为w(Ⅴ)=99.5%和w(Ⅱ)=99.3%。展开更多
The title complex was obtained by repeatly extracting the 0.1 mol/L HCI solution of PdCl2 with the petroleum ether in which p-CH3C6H4SC4H9 was previously dissolved at room temperature. The resulting precipitate, after...The title complex was obtained by repeatly extracting the 0.1 mol/L HCI solution of PdCl2 with the petroleum ether in which p-CH3C6H4SC4H9 was previously dissolved at room temperature. The resulting precipitate, after washed With deionized water and petroleum ether respectively,展开更多
文摘报道了9-[(4氟-)-3羟-基甲基丁基]鸟嘌呤(FHBG,Ⅱ)的改进合成方法,对起始原料喷昔洛韦(Ⅲ)的氨基和一个羟基用4-甲氧基氯化三苯甲烷保护,对另一个羟基磺酯化,得到N2-(p-甲氧基苯酰基二苯基甲基)-9-[(4甲-苯磺酰)-3-p-甲氧基苯酰基二苯基-甲氧基甲基丁基]鸟嘌呤(Ⅴ),收率为70.5%;再用四丁基氟化铵(TBAF)对化合物Ⅴ亲核取代4-甲苯磺酰基团,水解脱去保护基,即得FHBG。产品经1HNMR、IR、MS表征,并用HPLC分析了Ⅴ和Ⅱ,保留时间分别为5.89 m in和4.41 m in,积分计算质量分数分别为w(Ⅴ)=99.5%和w(Ⅱ)=99.3%。
基金This work was financially supported by the National Key Project for Basic Research(2010CB126102)the National Natural Science Foundation of China(30771427 and 31000884)+1 种基金the Natural Science Foundation of Heilongjiang Province,China(C201029)the Special Foundation for Scientific and Technological Innovation Research of Harbin(2011RFXXN038)
文摘The title complex was obtained by repeatly extracting the 0.1 mol/L HCI solution of PdCl2 with the petroleum ether in which p-CH3C6H4SC4H9 was previously dissolved at room temperature. The resulting precipitate, after washed With deionized water and petroleum ether respectively,