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1.
本文研究了1,10-双(1'-苯基-3'-甲基-5'-氧代吡唑-4'-基)癸二酮-[1,10](H2A)与1,10-菲罗啉(phen)或2,2'-联吡啶(dipy)对Co(Ⅱ)的协同萃取行为.确定了协萃配合物的组成为CoA·B(B分别为Phen和dipy),求得萃取平衡常数logKex分别是4.78(H2A+phen)和1.61(H2A+dipy),并对协萃配合物的IR谱进行了讨论.  相似文献   

2.
BPMOPP与1,10—菲咯啉对铈的协同萃取   总被引:3,自引:1,他引:3  
研究了1,2-双(1'-苯基-3'-甲基-5'-氧化吡唑-4'-基)-1,2苯二酮对盐酸介质中铈的萃取变价为及与1,10-菲咯啉从盐酸及盐与甲酸钠缓冲溶液中对铈的协同萃取得为,斜率法测定协萃合物的组成的CeA.HAphen,求得了协萃平衡常数,萃取法制得了固态配合物,对其组成,UV,IR,HNMR,TG-DTA进行了研究,讨论了协萃机理豚萃合物的可能结构。  相似文献   

3.
本文研究了1,10-双(1'-苯基-3'-甲基-5'-氧代吡唑-4'-基)癸二酮-[1,10](H2A)与1,10-菲罗啉(phen)或2,2'-联吡啶(dipy)对Co(Ⅱ)的协同萃取行为。确定了协萃配合物的组成为CoA.B(B分别为phen和dipy),求得萃取平衡常数logKex分别是4.78(H2A+phen)和1.61(H2A+dipy),并对协萃配合物的IR谱进行了讨论。  相似文献   

4.
研究了1,9-双(1-苯基-3-甲基-5-氧代吡唑-4-基)壬二酮-[1,9](BPMPND,H2A)与三辛基氧膦(TOPO,B)的氯仿溶液,从硝酸介质中对La(Ⅲ)、Dy(Ⅲ)的协同萃取,计算了体系的酸性协萃系数RA和协萃系数R,用斜率法测得协萃合物的组成为LaA·HA·B和DyA·HA·B,计算了协萃平衡常数,研究了温度对协萃反应的影响,用萃取法制得了固态协萃合物,并对其组成、IR及TG-DTA进行了研究.  相似文献   

5.
研究了1,9-双(1′-苯基-3′-甲基-5′-氧代吡唑-4′-基)壬二酮-(1,9)(BPMPND,H2A)与三辛基氧膦(TOPO,B)的氯仿溶液,从硝酸介质中对La(Ⅲ),Dy(Ⅲ)的协同萃取,计算了体系的酸性协萃系数RA和协萃系数R,用斜率法测得协萃合物的组成LaA.HA.B和DyA.HA.B计算了协萃取平衡常数,研究了温度对协萃反应的影响,用萃取法制得了固态协萃合物,并对其组成,IR及TG  相似文献   

6.
研究了1,10-双(1′-苯基-3′-甲基-5′-氧代吡唑-4-基)癸二酮-[1,10](BPMPDD,H2A)与三苯基氧化膦(TPPO,B)的氯仿溶液从硝酸介质中对Sm(Ⅲ)的协同萃取行为,计算了体系的酸性协萃系数RA和协萃系数R,用斜率法测得协萃合物的组成为SmA·HA·B,计算了协萃平衡常数,用萃取法制得了固态协萃合物,并对其组成、IR及TG-DTA进行了研究  相似文献   

7.
研究了1,10-双(1′-苯基-3′-甲基-5′-氧代吡唑-4-基)癸二酮-(1,10)(BPMPDD,H2A)与三苯基氧化膦(TPPO,B)的氯仿溶液从硝酸介质中对Sn(Ⅲ)的协同萃取行为,计算了体系的酸性协萃系数RA和协萃系数R,用斜率法测得协萃合物的组成为SmA.HA.B,计算了协萃平衡常数,用萃取法制得了固态协萃合物,并对其组成IR及TG-DTA进行了研究。  相似文献   

8.
杜家声 《应用化学》1995,12(5):58-61
研究了由4,4'-癸二酰-双-(1-苯基-3-甲基-5-吡唑啉酮)(DBPMP,简作H2A),氧化三辛基膦(TOPO),吡啶(Py)组成的三元体系从硝酸溶液中对铀的协同萃取,斜率法确定萃合物组成为UO2A.TOPO.Py,制取了固体协萃配合物,并用元素分析、IR及HNMR等进行了表征。  相似文献   

9.
苯基硫脲—磷酸三丁酯二元中性体系对钯的协同萃取研究   总被引:1,自引:1,他引:1  
陈淑群  卢业玉 《分析化学》1994,22(8):771-774
本文研究了苯基硫脲-磷酸三丁酯组成的二元中性体系在HCl介质中Pd(II)的萃取行为,发现该体系有明显的协同萃取效应。实验证明:在0.5-6mol/L HCl介质中,该体系能定量萃取Pd(II)。文中研究了萃取的最佳条件,试验了反萃取条件及共存离子对Pd(II)萃取的影响。用斜率法测得萃合物的组成为Pd:PTU:PTB=1:2:2,采用电子吸收光谱及红外光谱对协萃机理及萃合物的结构作了探讨。  相似文献   

10.
研究了新型双β-酮萃取剂2,6-双「(1-苯基-3-甲基-5-氧-4吡唑啉基甲酰基」吡啶的氯仿溶液对铀酰的萃取行为,所得萃合物组成为UO2(HA)2。  相似文献   

11.
用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.  相似文献   

12.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

13.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

14.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

15.
A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.  相似文献   

16.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

17.
A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.  相似文献   

18.
N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).  相似文献   

19.
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.  相似文献   

20.
In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.  相似文献   

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