N,N'-二乙氧拨基-O,O'-烷基二硫氨酯的合成及表征

由氯甲酸乙酯和硫氰酸钠经亲核取代反应和异构化合成N-烃氧羰基异硫氰酸酯中间体,再将该中间体与二醇经亲核加成反应合成了3种未见报道的N,N'-二乙氧羰基-0,O'-烷基二硫氨酯(1～3).经元素分析、红外光谱、核磁共振氢谱及碳谱分析,证实所合成的化合物即为目标产物.小型浮选实验结果表明,仅使用6g/t的目标化合物1～3,铜的品位即可分别达到6.12%,6.35%和5.92%,回收率分别达到75.31%,76.50%和76.35%,用量远低于丁基黄药,且铜的品位和回收率都有不同程度的提高,可作为一种新型捕收剂应用到硫化铜类矿物的浮选中.     

二苄基锡N,N-二甲基氨荒酸酯的合成及晶体结构

利用二苄基二氯化锡和N, N-二甲基氨荒酸钠反应, 合成了二苄基锡N, N-二甲基氨荒酸酯(C20H26N2S4Sn, Mr = 541.36)。通过元素分析、红外光谱、核磁共振氢谱和质谱对其结构进行了表征。用X-射线单晶衍射测定了该化合物的晶体结构。化合物为单斜晶系, 空间群P21/n, a = 1.3926(5), b = 0.9832(4), c = 1.7080(7) nm, b = 103.541(6), V = 2.274(2) nm3, Z = 4, Dc = 1.581 g/cm3, m(MoKa) = 1.500 mm-1, F(000) = 1096, R = 0.0482, wR = 0.1162. 在化合物的晶体中, 锡原子为六配位的畸变八面体构型。     

N,N'-二(糖基硫代亚脲基)芳基硫代膦酰二胺的合成

N;N'-二(糖基硫代亚脲基)芳基硫代膦酰二胺的合成;糖基异硫氰酸酯;硫代膦酰二肼;生物活性     

室温合成二硫化二正丁基黄原酸酯及其表征

以正丁醇、氢氧化钠和二硫化碳为原料,水作溶剂合成正丁基黄原酸钠,再与一氯化硫反应,室温条件下合成对称的二硫化二正丁基黄原酸酯,并探讨了反应条件对合成正丁基黄原酸钠和二硫化二正丁基黄原酸酯产率的影响。通过红外(FT-IR)、核磁(1H NMR)、质谱(MS)及元素分析等技术手段确定了产物的结构。优化的合成条件为:n(正丁基黄原酸钠)∶n(S2Cl2)=2∶1.1,温度为室温,溶剂为THF,反应时间为2 min,产率可达83.2%,反应条件温和,反应迅速、收率高。     

氮支冠醚二硫代甲酸酯化合物的合成

报道合成氮支冠醚的一种新连接方法。２，３－苯并－１０－氮杂－１，４，７，１３－四氧杂环十五－２－烯与二疏化碳在氢氧化钠存在下反应生成胺基二硫代甲酸盐，然后与卤代烃连接，形成单、双、叁冠醚。     

二苄基一氯化锡氨荒酸酯的合成与表征

合成了13个新的二苄基氯化锡氨荒酸酯化合物(PhCH_2)_2Sn(Cl)S_2CNRR＇。利用元素分析、UV.IR.H NMR谱和TG-DTA表征了它们的结构 初步生物活性研究表明,有些化合物表现出体外抑制白细胞P_(388)生长的活性。     

合成磷酰氯二烷基酯的新方法

以亚磷酸三烷基酯为原料,三氯异氰尿酸为氯代试剂,二氯甲烷为溶剂,在室温下合成了磷酰氯二烷基酯,其结构经1H NMR, 31P NMR和GC-MS确证.     

二苄基一氯化锡氨荒酸酯的合成与表征

合成了13个新的二苄基一氯化锡氨荒酸酯化合物(PhCH~2)~2Sn(Cl)Sn(Cl)S~2CNRR'。利用元素分析、UV、IR、^1HNMR谱和TG-DTA表征了它们的结构。初步生物活性研究表明,有些化合物表现出体外抑制白血细胞P~3~8~8生长的活性。     

水相中烷基硫代酯的绿色合成

发展了一种无需任何添加剂,在水相中合成烷基硫代酯的绿色方法.以卤代烃与硫代酰胺为原料,在水相中反应4 h,即可以较高收率得到预期产物,并可兼容多种官能团.与传统方法相比,该方法具有实验操作简单、反应绿色高效及原子经济等优点,并且可以实现克级制备,具有较高的应用价值.     

二苯基锗二硫代氨基甲酸酯的合成及表征

合成了10种二苯基锗二硫代氨基甲酸酯Ph2Ge(S2CNR2)2,用元素分析、IR、^1H NMR和MS表征了这些化合物的结构,体外实验表明,这些化合物对MCF－7,WiDr和EC癌细胞具有较的抑制活性。     

三苯基锗二硫代氨基甲酸酯的合成及表征

近年来 ,人们相继合成了有机锗倍半硫化物、有机锗硫杂环戊酮、含硫的螺环有机锗等化合Scheme1　 Synthetic route of compound物[1,2 ] .但烃基锗二硫代氨基甲酸酯类化合物尚未见报道 .我们 [3,4 ] 发现 ,有机锡二硫代氨基甲酸酯类化合物有很强的生物活性 .鉴于有机锗化合物比有机锡化合物毒性低得多 ,且副作用小 ,我们以三苯基氯化锗和二硫代氨基甲酸盐为原料 ,合成了一系列新型的有机锗含硫衍生物 (反应式如Scheme1所示 ) ,并对其结构进行了表征 ,初步生物活性测试结果表明 ,部分化合物显示出较强的抗癌活性 .1　实　　验1 .1　仪器与…     

三丁基锡二硫代氨基甲酸酯的合成及表征

通过三丁基氯化锡与二硫代氨基甲酸盐反应,合成了１０个 三丁基锡二硫代氨基甲酸酯,利用元素分析,ＩＲ、ＨＮＭＲ、ＵＶ和ＴＧ－ＤＴＡ表征了这些化合物结构,测定了部分化合物的生物活性。     

N,N’-二苯基-N,N’-二(9,9-二甲基芴-2-基)-9-己基-(4,4’-二胺基苯基)咔唑的合成方法及表征

以2,7-二溴咔唑为原料经过N-烷基化、Suzuki偶联反应、Buchwald-Hartwig偶联反应合成了有机发光二极管(OLED)空穴传输材料N,N’-二苯基-N,N’-二(9,9-二甲基芴-2-基)-9-己基-(4,4’-二胺基苯基)咔唑,利用NMR、IR和熔点等分析方法对产物结构进行了表征,并通过TG、UV-Vis及荧光光谱研究了物质的热稳定性和光学性能。     

Synthesis and Characterization of Homoleptic and Heteroleptic Complexes Involving Dithiocarbamates,Triphenylphosphine, and Nickel(II)

Abstract

Six new nickel complexes of two dithiocarbamate ligands (cyfdtc = N-cyclohexyl-N- furfuryldithiocarbamate and bztpedtc = N-benzyl-N-[2-thiophenylethyl]dithiocarbamate) namely, (Ni[cyfdtc]₂) (1), (Ni[bztpedtc]₂) (2), (Ni[cyfdtc][NCS][PPh₃]) (3), (Ni[bztpedtc] [NCS][PPh₃]) (4), (Ni[cyfdtc][PPh₃]₂)ClO₄ (5), and (Ni[bztpedtc][PPh₃]₂)ClO₄ (6) have been prepared and characterized using IR, electronic, and NMR (¹H and ¹³C) spectra. A single crystal X-ray structural analysis was carried out for complex 3 and showed that nickel is in a distorted square planar arrangement with the NiS₂PN chromophore. The shift in ν_C?N of the heteroleptic complexes to higher frequencies compared with the parent complex is assigned to mesomeric delocalization of electron density from the

dithiocarbamate ligand toward the metal atom, which increases the contribution of polar thioureide form in mixed ligand complexes. Electronic spectral studies suggest square planar geometry for the complexes. In the ¹³C NMR spectra, the upfield shift of NCS₂ carbon signal for 3 and 4 from the chemical shift value of 1 and 2 is due to effect of PPh₃ on the mesomeric drift of electron density toward nickel throughout thioureide C?N bond.     

Synthesis,Characterization, and in vitro Cytotoxicity of Gold(I) Complexes of 2‐(Diphenylphosphanyl)ethylamine and Dithiocarbamates

Gold(I) complexes of 2‐(diphenylphosphanyl)ethylamine or (2‐aminoethyl)diphenylphosphine (AEP), and dithiocaarbamates (R₂NCS₂) were prepared by the reaction of these ligands with (CH₃)₂S‐AuCl in dichloromethane. The synthesized complexes [Au(AEP)Cl] ( 1 ), [Au(AEP)₂]Cl ( 2 ), and [Au₂(R₂NCS₂)₂]_n (R₂ = dimethyl ( 3 ), diethyl ( 4 ), and dibenzyl ( 5 )) were characterized by elemental analysis, IR, ¹H, ¹³C and ³¹P NMR spectroscopy. The complexes were evaluated for anticancer activity against three cancer cells, A549 (human lung carcinoma), HCT15 (human colon cancer), and MCF7 (human breast cancer) cell lines. Three of the five tested complexes showed significant in vitro cytotoxicity and for A549, the inhibition effect of three compounds is greater than cisplatin.     

Synthesis, structural characterization, and fluorescent chemosensory properties of novel molecular clips based on diethoxycarbonyl glycoluril

A pair of novel fluorescent molecular clips was synthesized from diethoxycarbonal glycoluril cyclic ether and 1,2-dihydro-indazol-3-one. Their structures and conformations were confirmed by single crystal X-ray diffraction and chemosensory properties were studied by fluorescent spectroscope. Both of them exhibited selective recognition toward Fe³⁺ over other metal ions examined in DMF/CH₃OH (50:1, v/v).     

二苄基锡双氨荒酸酯的合成

由二苄基二氯化锡与氨荒酸盐反应，合成了１０个新的二苄基锡双氨荒酯化合物，利用元素分析，ＩＲ和＾１ＮＮＭＲ表征了这些化合物的结构。     

3-二甲胺基-N,N-二甲基丙酰胺的合成及表征

以甲醇钠为催化剂,甲醇为溶剂,丙烯酸甲酯和二甲胺为原料合成了3-二甲胺基-N,N-二甲基丙酰胺(DMDMAA).该方法的适宜工艺条件为:催化剂用量为丙烯酸甲酯质量的2.8%,反应温度为20~30℃,甲醇占初始反应液体积的50%.在此条件下,产品收率为62.8%,纯度达99.5%以上.通过红外光谱和质谱对其结构进行了表征.     

Synthesis and Structural Characterization of N,N-disubstituted Acylguanidines

A series of five N,N-disubstituted acylguanidines R~1C(O)N=C[N(H)R~2]NR_2~3(R~1=Mes or Ph; R~2=Ar??or Ar?; R~3=Cy, Bn, iPr, or Et)(Mes=2,4,6-Me_3C_6H_2, Ar??=2,6-iPr_2C_6H_3, Ar?=2,6-Me_2C_6H_3) was synthesized from the reactions of parent acylthioureas with respective secondary amines. According to structutral characterization by single-crystal X-ray diffraction, the rough reduction of the steric hindrance of R substitutents of R~1 C(O)N=C[N(H)R~2]NR_2~3(also abbreviated as R~1-R~2-R~3 for comparison purposes) led to the slight enlongation of N(1)–C(1) bond lengthes and small decrease of N(1)–C(1)–N(3) bond angles from Mes–Ar??–Cy(1) to Ph–Ar??–Bn(2), Ph–Ar??–iPr(3) and Ph–Ar?–Cy(4). At the same time, the N(1)–H(1)···O(1) intramolecular hydrogen bonds were observed in these cases. When R~3=Et, an interesting compound Ph-Ar?-Et(5) was obtained with the formation of intermolecular hydrogen bonds instead. 1 belongs to the monoclinic system, space group P2_(1/n) with a=9.6488(3), b=28.5318(8), c=11.9155(3) ?, b=91.439(2)o, V=3279.27(16) ?~3, and Z=4. 2 belongs to the triclinic system, space group P1 with a=9.6759(7), b=10.8613(8), c=15.7642(12) ?, a=70.429(3), b=79.257(4), g=69.052(4)o, V=1453.63(19) ?~3 and Z=2. 3 belongs to the monoclinic system, space group P2_(1/c) with a=11.1393(4), b=13.0643(4), c=17.6600(6) ?, b=101.866(2)o, V=2515.09(15) ?~3 and Z=4. 4 belongs to the monoclinic system, space group C2/c with a=17.8466(3), b=13.6126(2), c=21.6710(4) ?, b=90.7310(10)o, V=4992.72(14) ?~3 and Z=8. 5 is of orthorhombic system, space group P2_12_12_1 with a=10.5555(2), b=11.8913(2), c=14.9558(4) ?, V=1877.23(5) ?~3 and Z=4.