以异噁唑与硫酸二乙酯为原料,在碱性条件下一锅法合成了标题混合物。探讨了原料摩尔比、异噁唑溶液的组成、反应温度和提纯方式对收率的影响。确定了最佳工艺条件:n(异噁唑)∶n(硫酸二乙酯)∶n(NaOH)=1.285∶3.1∶3.1,其中原料异噁唑混...以异噁唑与硫酸二乙酯为原料,在碱性条件下一锅法合成了标题混合物。探讨了原料摩尔比、异噁唑溶液的组成、反应温度和提纯方式对收率的影响。确定了最佳工艺条件:n(异噁唑)∶n(硫酸二乙酯)∶n(NaOH)=1.285∶3.1∶3.1,其中原料异噁唑混合物中各组分含量为异噁唑、乙醇和水为15%∶71%∶14%。反应温度30℃,产品总收率91.6%。产物结构经1 H NMR表征。展开更多
3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Th...3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Thr with unprotected hydroxyl group on their side chain.Thus,DEPBT is useful for the synthesis of peptide alcohols,which have attracted much attention not only as the ligands but also as the enzyme inhibitors.A side reaction of DEPBT was found in the synthesis of Boc-β-Ala-HisOMe with unprotected imidazolyl group.In this paper,the discovery of this side reaction and the confirmation of the structure of this side product were reported.In addition,the influence of different reaction conditions on the side reaction were studied.Imidazolyl group was a key factor to cause the side reaction,excess DEPBT and high reaction temperature promoted the side reaction.展开更多
本文用3-氨基丙基三乙氧基硅烷(3-APTES)改性粘土岩,并通过X射线荧光光谱分析(XRF)、红外光谱仪(FT-IR)和扫描电子显微镜(SEM)对其进行了表征.结果显示,3-APTES改性粘土岩没有固定的表面结构,多为呈不规则多边型的薄片状晶体.以3-APTES...本文用3-氨基丙基三乙氧基硅烷(3-APTES)改性粘土岩,并通过X射线荧光光谱分析(XRF)、红外光谱仪(FT-IR)和扫描电子显微镜(SEM)对其进行了表征.结果显示,3-APTES改性粘土岩没有固定的表面结构,多为呈不规则多边型的薄片状晶体.以3-APTES改性粘土岩为吸附介质,探讨了反应时间、初始浓度、水相pH值、固液比、实验温度和离子种类等对该材料吸附U(Ⅵ)的影响.实验结果表明,pH为5、U(Ⅵ)初始浓度为50μg·mL^(-1)、固液比为1:200时,经过120 min 3-APTES改性粘土岩对U(Ⅵ)的吸附达到平衡,吸附效果最佳.升温有助于提高其吸附性能;溶液中Ca^(2+)、HCO_(3)^(-)、CO_(3)^(2-)等3种离子极大的抑制了3-APTES改性粘土岩的吸附性能.展开更多
文摘以异噁唑与硫酸二乙酯为原料,在碱性条件下一锅法合成了标题混合物。探讨了原料摩尔比、异噁唑溶液的组成、反应温度和提纯方式对收率的影响。确定了最佳工艺条件:n(异噁唑)∶n(硫酸二乙酯)∶n(NaOH)=1.285∶3.1∶3.1,其中原料异噁唑混合物中各组分含量为异噁唑、乙醇和水为15%∶71%∶14%。反应温度30℃,产品总收率91.6%。产物结构经1 H NMR表征。
文摘3-(Diethoxyphosphoryloxy)-1,2,3-benzotriazin-4(3H)-one(DEPBT) condensation developed by our group is an effective organophosphorus condensation reagent for the synthesis of protected peptides containing Tyr,Ser and Thr with unprotected hydroxyl group on their side chain.Thus,DEPBT is useful for the synthesis of peptide alcohols,which have attracted much attention not only as the ligands but also as the enzyme inhibitors.A side reaction of DEPBT was found in the synthesis of Boc-β-Ala-HisOMe with unprotected imidazolyl group.In this paper,the discovery of this side reaction and the confirmation of the structure of this side product were reported.In addition,the influence of different reaction conditions on the side reaction were studied.Imidazolyl group was a key factor to cause the side reaction,excess DEPBT and high reaction temperature promoted the side reaction.
文摘本文用3-氨基丙基三乙氧基硅烷(3-APTES)改性粘土岩,并通过X射线荧光光谱分析(XRF)、红外光谱仪(FT-IR)和扫描电子显微镜(SEM)对其进行了表征.结果显示,3-APTES改性粘土岩没有固定的表面结构,多为呈不规则多边型的薄片状晶体.以3-APTES改性粘土岩为吸附介质,探讨了反应时间、初始浓度、水相pH值、固液比、实验温度和离子种类等对该材料吸附U(Ⅵ)的影响.实验结果表明,pH为5、U(Ⅵ)初始浓度为50μg·mL^(-1)、固液比为1:200时,经过120 min 3-APTES改性粘土岩对U(Ⅵ)的吸附达到平衡,吸附效果最佳.升温有助于提高其吸附性能;溶液中Ca^(2+)、HCO_(3)^(-)、CO_(3)^(2-)等3种离子极大的抑制了3-APTES改性粘土岩的吸附性能.
