长链氨羧络合剂萃取稀土饵

研究了长链氨羧络合剂N,N′-二(十二烷基)乙二胺二乙酸钠(Na2R2Y)的氯仿溶液萃取稀土饵的行为;考察了溶液酸度、络合剂浓度、相比和温度对萃取率的影响.用摩尔比法测定了Na2R2Y与Er3+的络合摩尔比为1∶1;结果表明,Na2R2Y的氯仿溶液对饵的萃取率随络合剂浓度的增大而增大,随温度的升高而降低.     

N-烷基-α-亚胺基-丁二酸的新合成法

近年来β-氨基酸的化学研究引起人们很大的兴趣[1],它不仅是天然产物的一类重要的化合物,而且也具有医药开发价值.已知脯氨酸是一个α-亚氨基结构的,具有生理活性的天然氨基酸.本文研究了N-烷基-α-亚氨基-丁二酸4的合成方法和结构.通过糠醛的光氧化得到4-羟基丁内酯[2],后者在甲醇中缩醛化得到4-甲氧基丁内酯(1).化合物1与脂肪胺2在室温下通过Michael成可得到相应的加成产物3,进一步在HCl存在下用30%H2O2氧化开环得到目标产物4,如图Scheme 1所示.N-烷基-α-亚氨基-丁二酸(4)经元素分析,IR,1H NMR,13C NMR,MS以及X射线晶体衍射测定,确认了它们的结构.化合物4是一种二元酸,也可看作为β-亚氨基的二元酸,它们的生理活性有待进一步研究.     

对乙酰基偶氮羧光度法测铅铜合金中的痕量铅

２－（２－羧基苯偶氮）－７－（４－乙酰基苯偶氮）－１，８－二羟基－３，６－萘二磺酸（简称对乙酰基偶氮羧）是钡的高灵敏显色剂［１］，我们把对乙酰基偶氮羧用于铅的试验，结果发现，在ｐＨ＝２．０的酸性介质中，铅与显色剂形成兰色配合物，在λ＝７１５ｎｍ处有最...     

超共轭效应和同共轭效应计算与应用

超共轭效应和同共轭效应是有机化学中常用的一种定性的电子理论,但仅能笼统地解释一些反应现象,为了进一步理解这两种效应的含意,本文通过多电子共轭理论经验公式和CNDO/2计算探讨了这一电子理论。前一种方法能简便地计算出超共轭效应指数和同共轭效应指数,进而比较出基团间的微小差异;后一     

Crystal Structure and Spectroscopic Properties of[Ni（phen）3]Pic2.2CH3CN

1　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｔｈｅｐｒｏｃｅｓｓｏｆｔｈｅｐｒｅｐａｒａｔｉｏｎｏｆＮｉ(Ｐｉｃ) 2 Ｌ(Ｌ =1 ,3 ｂｉｓ (2 ｆｏｒｍｙｌｐｈｅｎｏｘｙ) 2 ｈｙｄｒｏｘｙｌ ｐｒｏｐａｎｅｔｈｉｏｓｅｍｉｃａｒｂａｚｏｎｅ )ｍｉｘｅｄｃｏｍｐｌｅｘｗｉｔｈｐｈｅｎ,ａｒｅｄｃｒｙｓｔａｌｗａｓｏｂｔａｉｎｅｄｉｎａｃｅｔｏｎｉｔｒｉｌｅｓｏｌｕｔｉｏｎ .Ｈｏｗｅｖｅｒ,ｔｈｅｅｌｅｍｅｎｔａｌａｎａｌｙｓｉｓｒｅｓｕｌｔｓｏｆｔｈｅｒｅｄｃｒｙｓｔａｌｉｎｄｉｃａｔｅｄｔｈａｔｉｔｉｓｎｏｔｔｈｅ…     

N-对甲苯磺酰β-丙氨酸镝配合物的合成、晶体结构及抑菌活性

稀土由于其特殊的电子结构,容易与一些中性、酸性和碱性生物配体形成配合物。本文合成并测定了对甲苯磺酰β-丙氨酸与稀土镝配合物的晶体结构及抑菌活性。     

A Valuable Synthetic Route to the Enantiopure Functionalized N-Substituted Aziridines

Chiral butyrolacto[3,4-b]-2(S)-6(R)-1-N-akylaziridines 7 were synthesized in enantiopure form utilizing racemic 5-methoxy-3-bromo-2(5H)-furanone (5) and available amines (6) as key precursors. After highly effective reduction of 7, the functionaiized 2(S),3(R)-dihyroxymethyl-N-alkylaziridines (8) were obtained in good yields with ≥98% ee. This is a simple and pratical method for the preparation of enantiopure aziridines which are important intermediates in the synthesis of biologic active molecules.     

Synthesis and Crystal Structure of 2-（N-Cyclohexyl）-imino-1,4-succinic Acid Dihydrate

1INTRODUCTIONItiswellknownthatthetwentyα-aminoacidsarethemostcommononesexistinginnature[1,.2]Actually,nineteenα-aminoacidsandoneα-iminoacidareutilizedinlivingcellsforproteinsynthesisunderthecontrolofgenes.Theyareinaspecialca-tegoryduetotheirfundamentalsofalllifeformsasbuildingblocksforlifeproteins[3～5].Aminoacidsarealsoimportantnaturalchiralmaterialsforsyn-thesizingpeptides,alkaloids,antibioticandmorecomplexmoleculeswithbiologicalactivities[6].Ac-cordingtothesyntheticmethodology,amino…     

新型手性<i>β</i>-烷氨基-<i>γ</i>-(<i>l</i>-孟氧基)丁内酯的合成

脂肪族伯胺作为亲核试剂与手性合成子5(R)-(l-孟氧基)-2(5H)-呋喃酮(4)发生不对称Michael加成反应, 得到一系列新的手性β-烷氨基-γ-(l-孟氧基)丁内酯类化合物6(产率34～81%, de≥98%). 通过IR, ¹H NMR, ¹³C NMR, MS, 元素分析及单晶X射线衍射分析, 确认了它们的化学结构、立体化学和绝对构型. 此结果为某些具有生物活性化合物及复杂分子的合成提供了新的途径.     

Synthesis and Crystal Structure of Spiro[1-bromo-4-l-menthyloxy-5-oxo-6-oxa-bicyclo [3.1.0] hexane-2,2''''-3''''-(16''''-methoxyacetatyl-4''''-l-menthyloxybutyrolactone)]

The title compound,spiro[1-bromo-4-l-menthyloxy-5-oxo-6-oxa-bicyclo[3.1.0]-hexane-2,2'-3'-(16'-methoxyacetatyl-4'-l-menthyloxybutyrolactone)] 1,was obtained via tandem asymmetric double Michael addition/internal nucleophilic substitution of the chiral synthon,5-l-menthyloxy-3-bromo-2-(5H)-furanone 2 with methoxy α-chloroacetate as a nucleophile under mild conditions,and structurally determined by single-crystal X-ray diffraction.Crystal data:C31H47BrO9,Mr = 643.60,orthorhombic,space group P212121,a = 9.6564(7),b = 14.8994(11),c =23.6771(17) (A),V= 3406.5(4) (A)3,Z= 4,Dc= 1.255 g/cm3,λ(MoKα) = 0.71073(A),μ= 1.254 mm-1and F(000) = 1360.The structure was refined to R =0.0324 and wR = 0.0737 for 5123 observed reflections (I ＞ 2σ(I)).The crystallographic results of molecule 1 show that the interesting reaction of 2 with methoxy α-chloroacetate,in the usual manner,gave the spiro-cyclopropane skeleton with O-linked derivative containing multiple stereogenic centers 1 rather than the expected C-linked derivative.