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3-三氯锡基丙酸酯及其配合物的合成与结构表征
引用本文:田来进,俞庆森,刘希杰,商志才,王涛,赵文娜. 3-三氯锡基丙酸酯及其配合物的合成与结构表征[J]. 有机化学, 2003, 23(5): 441-446
作者姓名:田来进  俞庆森  刘希杰  商志才  王涛  赵文娜
作者单位:1. 浙江大学化学系,杭州,310027;曲阜师范大学化学系,曲阜,273165
2. 浙江大学化学系,杭州,310027
3. 曲阜师范大学化学系,曲阜,273165
4. 中国科学院上海有机化学研究所,上海,200032
基金项目:国家自然科学基金 (No.2 0 1 730 50 )资助项目 .
摘    要:合成了4个新的3-三氯锡基丙酸酯Cl3SnCH2CH2COOR(R=环戊基,1;环己基,2 ;环戊甲基,3;环己甲基,4),并通过其与二丁基亚砜(L^1)、2,2’-联吡啶 (L^2)、1,10-菲咯啉(L^3)的低热固相反应合成了6个相应的配合物 Cl3SnCH2CH2COOR·L(L=L^1,a;L^2,b;L^3,c).利用元素分析、红外光谱、核磁共振 对其结构进行了表征,并通过X射线单晶衍射测定了1和2的晶体结构,二者均为具 有分子内羰基氧原子配位的畸变三角双锥结构.1属于单斜品系,空间群P21/c, a=0.9842(2)nm,b=1.0923(8)nm,c=1.23948(11)nm,β=93.894(15)°,V=1.3294(4) nm^3,Mr=366.23,Z=4.2属于单斜晶系,空间群P21/c,a=1.04443(9)nm,b=1.04823 (7)nm,c=1.28113(9)nm,β=90.953(8)°,V=1.40239(19)nm^3,Mr=380.25,Z=4.

关 键 词:结构表征  有机锡化合物  晶体结构  丙酸酯  抗癌药  联吡啶 P  二氮杂菲 P  元素分析  红外分光光度法  质子磁共振谱法
修稿时间:2002-03-21

Synthesis and Structural Characterization of 3- Trichlorostannylpropionates and Their Complexes
TIAN,Lai-Jin a,b YU,Qing-Sen,a LIU,Xi-Jieb SHANG,Zhi-Caia WANG,Taoc ZHAO,Wen-Naa. Synthesis and Structural Characterization of 3- Trichlorostannylpropionates and Their Complexes[J]. Chinese Journal of Organic Chemistry, 2003, 23(5): 441-446
Authors:TIAN  Lai-Jin a  b YU  Qing-Sen  a LIU  Xi-Jieb SHANG  Zhi-Caia WANG  Taoc ZHAO  Wen-Naa
Affiliation:Department of Chemistry,Zhejiang University;department of Chemistry, Qufu Normal University;Shanghai Institute of Organic Chemistry,Chinese Academy of sciences
Abstract:The synthesis and characterization by means of elemental analysis, IR, NMR spectra of 3-trichlorostannylpropionates, Cl3SnCH2CH2COOR (R = cyclopentyl, 1; cyclohexyl, 2; cyclopentylmethyl, 3; cyclohexylmethyl, 4), are described together with their complexes with dibutylsulfoxide (L1). 2,2'-bipyridyl (L ) and 1,10-phenanthroline (L3), Cl3SnCH2CH2COORo L (L= L1, a; L2, b; L3, c), formed by low-heating solid-state reaction. The crystal structures of 1 and 2 show that the tin atom adopts a distorted trigonal bipyramid geometry via intramolecular carbonyl oxygen to tin coordination [the distances of Sn-0 bond are 0.2351(6) ran for 1 and 0.2362(3) nm for 2]]. Compound 1 belongs to monoclinic with space group P2]/c, a = 0.9842(2) nm, b =1. 0923(8) nm, c = 1.23948(11) nm, /? = 93.894(15)°, V= 1.3294(4) ran3, Mr = 366.23, 7 = 4. Compound2 belongs to monoclinic with space group P2{/c, a = 1.04443(9) nm, b = 1.04823(7) nm, c = 1.28113(9) nm, / = 90. 953(8)°, V= 1.40239(19) nm3, Mr = 380.25, Z = 4
Keywords:organotin(IV) complex   solid-state reaction   3-trichlorostannylpropinnate   crystal structure
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