CN108467359A - 一种铜配合物 - Google Patents
一种铜配合物 Download PDFInfo
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- CN108467359A CN108467359A CN201810364052.5A CN201810364052A CN108467359A CN 108467359 A CN108467359 A CN 108467359A CN 201810364052 A CN201810364052 A CN 201810364052A CN 108467359 A CN108467359 A CN 108467359A
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- 150000004699 copper complex Chemical class 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000010189 synthetic method Methods 0.000 claims abstract description 5
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical class O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- 238000010992 reflux Methods 0.000 claims abstract description 4
- 229940117360 ethyl pyruvate Drugs 0.000 claims abstract description 3
- 239000000706 filtrate Substances 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- -1 ethyl pyruvate Nitrile Chemical class 0.000 claims description 3
- 238000002447 crystallographic data Methods 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims 1
- XXRCUYVCPSWGCC-UHFFFAOYSA-N Ethyl pyruvate Chemical compound CCOC(=O)C(C)=O XXRCUYVCPSWGCC-UHFFFAOYSA-N 0.000 abstract description 3
- 150000002825 nitriles Chemical class 0.000 abstract description 3
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 abstract 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 150000001414 amino alcohols Chemical class 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000005160 1H NMR spectroscopy Methods 0.000 description 3
- JAWGVVJVYSANRY-UHFFFAOYSA-N cobalt(3+) Chemical class [Co+3] JAWGVVJVYSANRY-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001879 copper Chemical class 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical class Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 238000007333 cyanation reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 1
- XUEWIQNQPBSCOR-UHFFFAOYSA-N 2-nitro-1-phenylethanol Chemical class [O-][N+](=O)CC(O)C1=CC=CC=C1 XUEWIQNQPBSCOR-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 description 1
- 238000009876 asymmetric hydrogenation reaction Methods 0.000 description 1
- 150000003935 benzaldehydes Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- GSOLWAFGMNOBSY-UHFFFAOYSA-N cobalt Chemical compound [Co][Co][Co][Co][Co][Co][Co][Co] GSOLWAFGMNOBSY-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical class C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/79—Acids; Esters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2217—At least one oxygen and one nitrogen atom present as complexing atoms in an at least bidentate or bridging ligand
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/79—Acids; Esters
- C07D213/803—Processes of preparation
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- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0213—Complexes without C-metal linkages
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/10—Complexes comprising metals of Group I (IA or IB) as the central metal
- B01J2531/16—Copper
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Abstract
一种铜配合物，其化学式如下：
Description
一、技术领域
本发明涉及一种新化合物及其制备方法，特别涉及一种铜化合物及其制备方法，确切地说是一种配合物的制备及合成方法。
二、背景技术
铜配合物是重要的催化剂和医药化工产品，其作为催化剂在二乙基锌与苯甲醛对映选择性加成反应等反应中有较好的催化效果。【1-5】
参考文献：
1.Asymmetric hydrogenation catalyzed by bis(dimethylglyoximato)cobalt(II)-achiral base complex and chiral amino alcohol conjugatedsystems.Oxidoreductase model with enantioselectivity ，Ohgo, Yoshiaki; Natori,Yukikazu; Takeuchi, Seiji; Yoshimura, Juji , Chemistry Letters (1974), (11),1327-30.
Synthesis, structure and acid-base properties of cobalt(III) complexeswith aminoalcohols tepanenko, O. N.; Reiter, 2. L. G. Ukrainskii KhimicheskiiZhurnal (Russian Edition), (1992), 58(12), 1047-54.
3. Cobalt(III) mono- and trinuclear complexes with O,N-chelatingaminoalcohols apanadze, T. Sh.; Gulya, A. P.; Novotortsev, V. M.; Ellert, O.G.; Shcherbakov, V. M.; Kokunov, Yu. V.; Bushaev, Yu. A. KoordinatsionnayaKhimiya (1991), 17(7), 934-40.
4. Magnetic properties of cobalt complexes with amino alcohols, Evreev,V. N.; Bogdanov, A. P. 13 Vses. Chugaev. Soveshch. po Khimii Kompleks.Soedin., 1978 (1978), 137.
5.Synthesis, stereochemistry, and reactions of cobalt(III) complexes withamino alcohol ligands
Okamoto, Martha S. No Corporate Source data available |(1974), 146 pp.
6.Synthesis and properties of isomeric tris(N-[2-hydroxyethyl]ethylenediamine)cobalt(III) and tris(N-[2-hydroxypropyl]ethylenediamine)cobalt(III) chlorides, arpeiskaya, E. I.; Kukushkin, Yu. N.; Trofimov, V. A.;Yakovlev, I. P. , Zhurnal Neorganicheskoi Khimii (1971), 16(7), 1960-4。
三、发明内容
本发明旨在提供含配合物，所要解决的技术问题是一步合成得到目标产物。
本发明所称的铜配合物是由3-羟基-2-吡啶羧酸与二水合氯化铜制备的由以下化学 式所示的配合物：
化学名称：双[3-羟基-2-吡啶羧酸]铜配合物,简称配合物(I)。
该配合物在丙酮酸乙酯的亨利反应及苯甲醛的腈硅化反应中显示了一定的催化性能，其转化率分别达92%及99%。
本合成方法包括合成和分离，所述的合成是称取0.2002g 3-羟基-2-吡啶羧酸放入100mL圆底烧瓶中，加入50mL无水甲醇并搅拌使其溶解；将0.1227g氯化铜加入上述溶液，加热回流48h；反应结束后趁热过滤反应溶液，滤液自然挥发，数天后有晶体析出。
合成反应如下：
本合成方法一步得到目标产物，工艺简单，操作方便。
该反应的反应机理可推测为两分子的3-羟基-2-吡啶羧酸在二水合氯化铜的作用下脱去两分子氯化氢，一步形成双双[3-羟基-2-吡啶羧酸]铜配合物。
四、附图说明
图1：双[3-羟基-2-吡啶羧酸]铜配合物的单晶X-衍射图。
五、具体实施方式
铜配合物的制备：
称取0.2002g3-羟基-2-吡啶羧酸放入100mL圆底烧瓶中，加入50mL无水甲醇并搅拌使其溶解；将0.1227g氯化铜加入上述溶液，加热回流48h；反应结束后趁热过滤反应溶液，滤液自然挥发，数天后有晶体析出。
将晶体用石油醚和正己烷冲洗3次，真空干燥30min，得目标产物，产率为63%，熔点216-218°C; 元素分析数据C12 H8CuN2 O6，理论值：C： 42.3%； H：2.4%；N：8.24%； 实测值：C42.01%； H：3.03%；N：8.11%；红外光谱数据(KBr, cm-1)：3941；3395；3038；2769；1801；1619；1438；1387；1285；964；826；746；622；
铜配合物的晶体数据：
经验式 C12H8CuN2O6
分子量 339.74
温度 293（2）K
波长 0.71073 Å
晶系， 空间群 单斜晶系,P 21/c
晶胞参数 a = 6.3682(12) Å alpha = 90°.
b = 11.416 (2) Å beta = 91.928(4)°.
c = 8.0503(15) Å gamma = 90°.
体积 584.91((19) Å^3
电荷密度 2,1.929 g/m^3
吸收 校正参数 1.900 mm^-1
单胞内的电子数目 342
晶体大小 0.170x 0.120x 0.100mm
Theta 角的范围 3.098 to 25.490°
HKL的指标收集范围 -7<=h<=7, -10<=k<13, -9<=l<=9
收集/独立衍射数据 3257/1090[R(int) = 0.0363]
theta = 30.5的数据完整度 99.9 %
吸收校正的方法 多层扫描
精修使用的方法 F^2 的矩阵最小二乘法
数据数目/使用限制的数目/参数数目 1090/0/101
精修使用的方法 1.099
衍射点的一致性因子 R1 = 0.0461，wR2= 0.093
可观察衍射的吻合因子 R1 = 0.0567, wR2 = 0.1157
差值傅里叶图上的最大峰顶和峰谷 0.585 and -0.278e.Å^-3
晶体典型的键长数据：
Cu(1)-O(2)#1 1.949(3)
Cu(1)-O(2) 1.949(3)
Cu(1)-N(1)#1 1.965(3)
Cu(1)-N(1) 1.966(3)
N(1)-C(6) 1.323(4)
N(1)-C(2) 1.349(5)
O(1)-C(1) 1.229(5)
O(2)-C(1) 1.279(5)
O(3)-C(3) 1.344(5)
O(3)-H(3) 0.64(4)
C(1)-C(2) 1.501(5)
C(2)-C(3) 1.393(5)
C(3)-C(4) 1.389(5)
C(4)-C(5) 1.367(5)
C(4)-H(4) 0.9300
C(5)-C(6) 1.387(5)
C(5)-H(5) 0.9300
C(6)-H(6) 0.9300
晶体典型的键角数据
O(2)#1-Cu(1)-O(2) 180.0
O(2)#1-Cu(1)-N(1)#1 83.91(11)
O(2)-Cu(1)-N(1)#1 96.09(11)
O(2)#1-Cu(1)-N(1) 96.09(11)
O(2)-Cu(1)-N(1) 83.91(11)
N(1)#1-Cu(1)-N(1) 180.0
C(6)-N(1)-C(2) 119.3(3)
C(6)-N(1)-Cu(1) 129.7(3)
C(2)-N(1)-Cu(1) 110.8(2)
C(1)-O(2)-Cu(1) 114.3(2)
C(3)-O(3)-H(3) 105(4)
O(1)-C(1)-O(2) 126.5(3)
O(1)-C(1)-C(2) 118.6(3)
O(2)-C(1)-C(2) 114.9(3)
N(1)-C(2)-C(3) 121.7(3)
N(1)-C(2)-C(1) 115.3(3)
C(3)-C(2)-C(1) 123.0(3)
O(3)-C(3)-C(4) 120.9(3)
O(3)-C(3)-C(2) 121.1(3)
C(4)-C(3)-C(2) 118.0(4)
C(5)-C(4)-C(3) 119.8(3)
C(5)-C(4)-H(4) 120.1
C(3)-C(4)-H(4) 120.1
C(4)-C(5)-C(6) 118.9(3)
C(4)-C(5)-H(5) 120.5
C(6)-C(5)-H(5) 120.5
N(1)-C(6)-C(5) 122.2(4)
N(1)-C(6)-H(6) 118.9
C(5)-C(6)-H(6) 118.9
O(1)-Cu(1)-Cu(1)#1 84.60(7)
亨利反应应用
2-硝基-1-苯基乙醇
称取0.0255g（0.075mmol）配合物，置于25mL 的小烧瓶中，加入1mL 甲醇，再向溶液中加入0.15mL丙酮酸乙酯和0.25mL硝基甲烷，常温下搅拌反应6小时后，进行1HNMR检测, 其转化率为：92%;1 H NMR (CDCl 3 ): δ ) 4.86 (d,J =13.8 Hz, 1H), 4.58 (d, J =13.8Hz, 1H), 4.34 (m, 2H), 3.85(s, 1H), 1.46 (s, 3H), 1.33 (t, J ) 7.2 Hz, 3H).13C NMR (CDCl 3 ):δ=173.4, 80.9, 72.4, 63.0, 23.8, 13.9。
硅腈化反应
硅腈化反应也是一种常用的有机合成反应，是合成手性腈醇一种重要方法。在有机医药中间体方面也有广泛的应用。
实验的反应方程式：
称取0.0548g（0.1mmol）配合物，置于25mL小烧瓶中，加入2mLDMSO，再向溶液中加入0.1mL苯甲醛和0.3mL三甲基硅腈，常温下搅拌72h，进行1HNMR检测; 催化转化率: >99%;1HNMR (300MHz, CDCl3) 7.56–7.59 (m, 0.9 Hz, 2H), 7.31–7.34 (m, 3H), 5.43 (s,1H), 0.16 (s, 9H). 13C NMR (75 MHz, CDCl3) 136.1, 128.8(x2), 126.2(x2), 119.1,63.5, -0.39(x3)。
Claims (4)
1.一种铜配合物，其化学式如下：
2.权利要求1所述的铜配合物，在293 K 温度下，在牛津X-射线单晶衍射仪上，用经石墨单色器单色化的MoKα射线,λ=0.71073 Å以ω-θ扫描方式收集衍射数据，其特征在于晶体属单斜晶系,P 21/c晶胞参数: a = 6.3682(12) Å alpha = 90°；b = 11.416 (2) Å beta= 91.928(4)°；c = 8.0503(15) Å gamma = 90°。
3.权利要求1所述的铜配合物的合成方法，包括合成和分离，所述的合成是称取0.2002g3-羟基-2-吡啶羧酸放入100mL圆底烧瓶中，加入50mL无水甲醇并搅拌使其溶解；将0.1227二水合氯化铜加入上述溶液，加热回流48h；反应结束后趁热过滤反应溶液，滤液自然挥发，数天后有晶体析出。
4.权利要求1所述的铜配合物的用途，是该配合物在丙酮酸乙酯的亨利反应及苯甲醛的腈硅化反应中显示了一定的催化性能，其转化率分别达92%及99%。
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| CN104610284A (zh) * | 2015-03-10 | 2015-05-13 | 合肥工业大学 | 一种铜配合物 |
| CN105669772A (zh) * | 2016-02-23 | 2016-06-15 | 合肥祥晨化工有限公司 | 一种镍配合物的制备及其合成方法 |
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| CN104610284A (zh) * | 2015-03-10 | 2015-05-13 | 合肥工业大学 | 一种铜配合物 |
| CN105669772A (zh) * | 2016-02-23 | 2016-06-15 | 合肥祥晨化工有限公司 | 一种镍配合物的制备及其合成方法 |
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