NbCl3(1,2-dimethoxyethane)(MeC.tplbond.CMe) | 126083-92-9

• 分子结构分类: 有机化合物 - 有机氧化合物
• 英文名称: NbCl3(1,2-dimethoxyethane)(MeC.tplbond.CMe)
• 英文别名: NbCl3(1,2-dimethoxyethane)(MeCCMe)；NbCl3(dme)(MeCCMe)；but-2-yne;1,2-dimethoxyethane;trichloroniobium
• CAS: 126083-92-9
• 化学式: C₈H₁₆Cl₃NbO₂
• 分子量: 343.479
• InChiKey: OBKMSNSYUNSSEY-UHFFFAOYSA-K

计算性质

• 辛醇/水分配系数(LogP)：
  None
• 重原子数：
  None
• 可旋转键数：
  None
• 环数：
  None
• sp3杂化的碳原子比例：
  None
• 拓扑面积：
  None
• 氢给体数：
  None
• 氢受体数：
  None

反应信息

• 作为反应物：
  描述：

  NbCl3(1,2-dimethoxyethane)(MeC.tplbond.CMe) 、 bis(5-(trimethylsilyl)-1H-pyrazol-1-yl)methane 以 二氯甲烷 为溶剂， 以82%的产率得到[NbCl3(bis(5-trimethylsilylpyrazol-1-yl)methane)(MeC.tplbond.CMe)]* 0.5 CH2Cl2
  参考文献：
  名称：

  Synthesis, spectroscopic characterization and dynamic behaviour of niobium complexes with poly(pyrazol-1-yl)methane ligands

  摘要：

  The complex [{NbCl3(dme)}(n)] 1 (dme = 1,2-dimethoxyethane) reacted with an excess of bis(pyrazol-1-yl)methane (bzpm), bis(3.5-dimethylpyrazol-1-yl)methane (bdmpzm) or bis(5-trimethylsilylpyrazol-1-yl)methane (btpzm) to give the binuclear complexes [{NbCl3(bpzm)}(2)] 2, [{NbCl3(bdmpzm)}(3)] 3 and [{NbCl3(btpzm)}(2)] 4, respectively. Mononuclear acetylene complexes [NbCl3(L-L)(RC drop CR')] (R = R' = Ph, L-L = bpzm 5, bdmpzm 6 or btpzm 7; R = R' = CO(2)Me, L-L = btpzm 8; R = R' = Me, L-L = bpzm 9, bdmpzm 10 or btpzm 11) have been prepared from either the reaction of 2-4 with acetylenes or the interaction of acetylene complexes [NbCl3(dme)(RC drop CR')] with the appropriate L-L. This last reaction with tris(pyrazol-1-yl)methane (tpzm) or tris(3,5-dimethylpyrazol-1-yl)methane (tdmpzm) in the presence of 1 equivalent of AgBF4 afforded the cationic complexes [NbCl2(L-L-L)(RC drop CR')]BF4 (R = R' = Ph, L-L-L = tpzm 12 or tdmpzm 13; R = R' = Me, L-L-L = tpzm 14 or tdmpzm 15). The structures of these complexes have been determined by spectroscopic methods. Variable-temperature NMR studies of some of the complexes were carried out in order to establish their fluxional behaviour in solution and free activation energy values were calculated at the coalescence temperature.

  DOI：

  10.1039/dt9950001015
• 作为产物：
  描述：

  2-丁炔 、 1,2-二甲氧基乙烷-三氯铌(1:1) 以 二氯甲烷 为溶剂， 以51%的产率得到NbCl3(1,2-dimethoxyethane)(MeC.tplbond.CMe)
  参考文献：
  名称：

  三卤化铌炔烃配合物的合成与表征

  摘要：

  DOI：

  10.1021/om00119a010

文献信息

• Niobium complexes containing a new chiral heteroscorpionate ligand and the reactivity of such a complex with O2 to give the first gem-diolate niobium complex
  作者：A. Otero、J. Fernández-Baeza、A. Antiñolo、J. Tejeda、A. Lara-Sánchez、L. Sánchez-Barba、M. T. Expósito、A. M. Rodríguez

  DOI：10.1039/b300497j

  日期：2003.4.4

  R′ = Me, 5; R = Ph, R′ = Et, 6). The structures of these complexes have been determined by spectroscopic methods. Variable-temperature NMR studies of these complexes were carried out in order to study their dynamic behaviour in solution. The barriers to alkyne rotation have also been calculated. The reactivity of [NbCl2(dpmpza)(Me3SiCCSiMe3)], 4, toward molecular oxygen is particularly noteworthy since

  新型不对称双（吡唑-1-基）的合成 配体，（3,5-二苯基吡唑-1-基-3'，5'-二甲基吡唑-1-基）甲烷（dpmpzm），1进行了研究。去质子化亚甲基用Bu n Li制备1，然后与二氧化碳反应得到[Li（dpmpza）（H 2 O）} 4 ]，2 [dpmpza =（3,5-二苯基吡唑-1-基-3' ，5'-二甲基吡唑-1-基）乙酸盐]，这是一种新型的手性单阴离子NNO三脚架配体。该化合物是引入这种蝎子的极好的前体配体过渡金属配合物。络合物[NbCl 3（dme）（RC CR'）]（dme =1,2-二甲氧基乙烷）与反应2，得到对应的[NbCl 2（dpmpza）（RC CR'）]配合物（R = R'= Me中，3 ; R = R'=森达3，4 ; R =苯基，R'=我，5 ; R = Ph，R'= Et，6）。这些配合物的结构已经通过光谱法确定。变温NMR为了研究它们在溶液中的动态
• Phosphorus ylide-containing niobium complexes: preparation and characterization of homo- and heteronuclear compounds with an α -keto ylide ligand
  作者：A. Antiñolo、F. Carrillo-Hermosilla、E. Dı́ez-Barra、J. Fernández-Baeza、A. Lara-Sánchez、A. Otero、J. Tejeda

  DOI：10.1016/s0022-328x(98)00811-0

  日期：1998.11

  [NbCl3(dme)(RCCR′)] with a heterocycle containing α-keto stabilized phosphorus ylide, 2-TCMP=[2-thiazolylcarbonyl}methylene]triphenylphosphorane, and these reactions give the α-keto ylide-containing niobium complexes [NbCl3(2-TCMP)}2] (1) and [NbCl3(2-TCMP)(RCCR′)], R=R′=Ph (2); R=R′=Me (3); R=R′=Et (4); R=Ph, R′=Me (5); R=Ph, R′=Et (6); R=Ph, R′=Pr (7); R=Ph, R′=SiMe3 (8), respectively. The reactivity of 5 towards

  已经研究了[NbCl 3（dme）} n ]或[NbCl 3（dme）（RCCR'）]与含有α-酮稳定的磷内酯的杂环的反应，2-TCMP = [2-噻唑基羰基}亚甲基]三苯基膦烷，这些反应得到了含α-酮基内酯的铌配合物[NbCl 3（2-TCMP）} 2 ]（1）和[NbCl 3（2-TCMP）（RCCR'）]， R = R'= Ph（2）; R = R'= Me（3）; R = R'= Et（4）; R ＝ Ph，R′＝ Me（5）；R = Ph，R'= Et（6）；R ＝ Ph，R′＝ Pr（7）；R = Ph，R'= SiMe 3（8）。还研究了5对不同试剂的反应性。化合物5与MeLi反应，通过苯环的去质子化过程，得到邻金属化的配合物[N 6 H 4）-O，N}] 2（9），而炔炔配体损失了。此外，5与[AuPPh 2 R] CF 3 SO 3和AgCF 3 SO 3反应，得到杂金属络合物[NbCl
• A new type of monoanionic “scorpionate” ligand. Synthesis, spectroscopic characterisation and dynamic behaviour of some niobium(III) complexes
  作者：Antonío Otero、Juan Fernández-Baeza、Juan Tejeda、Antonío Antiñolo、Fernando Carrillo-Hermosilla、Enrique Díez-Barra、Agustin Lara-Sánchez、María Fernández-López

  DOI：10.1039/b002742l

  日期：——

  The syntheses of novel scorpionate ligands in the form of the lithium derivative [Li(H2O)(bdmpza)}4] 1 [bdmpza = bis(3,5-dimethylpyrazol-1-yl)acetate] or as the alcohol derivative 2,2-bis(3,5-dimethylpyrazol-1-yl)ethanol 2 (Hbdmpze) have been studied. These compounds are excellent precursors for the introduction of these scorpionate ligands into transition metal complexes. The complex [NbCl3(dme)}n] (dme = 1,2-dimethoxyethane) reacted with 1 and 2, the latter with prior addition of BunLi, to give the binuclear complexes [NbCl2(bdmpzx)}2] (x = a, 3; x = e, 4) [bdmpze = 2,2-bis(3,5-dimethylpyrazol-1-yl)ethoxide]. Complex 3 reacted with 1 to give the complex [NbCl(bdmpza)2}2] 5. In the same way the reaction of the mononuclear species [NbCl3(dme)(RCCR′)] with 1 and 2, the latter with prior addition of BunLi, gave the appropriate [NbCl2(bdmpzx)(RCCR′)] complexes [x = a, R = R′ = Me, 6; Et, 7; Ph, 8; or SiMe3, 9; R = Ph, R′ = Me, 10; R = Ph, R′ = Et, 11; R = Ph, R′ = SiMe3, 12; x = e, R = R′ = Me, 13; Et, 14; or Ph, 15; R = Ph, R′ = Me, 16; R = Ph, R′ = Et, 17; R = Ph, R′ = SiMe3, 18]. The structures of these complexes have been determined by spectroscopic methods. Variable-temperature NMR studies were carried out in order to study their dynamic behaviour in solution. The barriers to alkyne rotation have also been calculated. Reaction of 10 with LiCp′ (Cp′ = C5H4SiMe3) gave the mixed Cp–bdmpza complex [NbCp′Cl(bdmpza)] 19.

  研究人员合成了锂衍生物 [Li(H2O)(bdmpza)}4] 1 [bdmpza =双(3,5-二甲基吡唑-1-基)乙酸酯] 或醇衍生物 2,2-双(3,5-二甲基吡唑-1-基)乙醇 2 (Hbdmpze) 形式的新型蝎酸盐配体。这些化合物是将这些蝎酸配体引入过渡金属配合物的极佳前体。络合物 [NbCl3(dme)}n] （dme = 1,2-二甲氧基乙烷）与 1 和 2（后者事先加入了 BunLi）反应，得到双核络合物 [NbCl2(bdmpzx)}2] （x = a, 3; x = e, 4）[bdmpze = 2,2-双（3,5-二甲基吡唑-1-基）乙醇]。络合物 3 与 1 反应生成络合物 [NbCl(bdmpza)2}2] 5。同样，单核物质[NbCl3(dme)(RCCRâ²)]与 1 和 2（后者事先加入了 BunLi）反应，得到了相应的[NbCl2(bdmpzx)(RCCRâ²)]络合物[x = a，R = Râ²Â = Me，6；Et，7；Ph，8；或 SiMe3，9；R = Ph，Râ²Â = Me，10；R = Ph，Râ²Â = Et，11；R = Ph，Râ²Â = SiMe3，12；x = e，R = Râ²Â = Me，13；Et，14；或 Ph，15；R = Ph，Râ²Â = Me，16；R = Ph，Râ²Â = Et，17；R = Ph，Râ²Â = SiMe3，18]。这些复合物的结构已通过光谱方法确定。为了研究它们在溶液中的动态行为，还进行了变温核磁共振研究。还计算了炔旋转的障碍。10 与 LiCpâ²（Cpâ² = C5H4SiMe3）反应生成了混合 Cpâbdmpza 复合物 [NbCpâ²Cl(bdmpza)] 19。
• Amine−Phenolate Ligands in Niobium Chemistry: π-Interactions Probed by an Ancillary Alkyne Ligand
  作者：Emmanuelle Despagnet-Ayoub、Sophie Schigand、Laure Vendier、Michel Etienne

  DOI：10.1021/om801139m

  日期：2009.4.13

  A series of alkyne niobium complexes based on tetrapodal amine bis(phenolato) ligands NbCl[ONNO]R(MeCCMe) ([ONNO]R = N(CH2CH2NMe2)2(CH2C6H2-3,5-R2-2-O), R = H, Me) (4), and tripodal amine phenolato ligands NbCl2[ONN]Me(MeCCMe) ([ONN]Me = NMe(CH2CH2NMe2)(CH2C6H2-3,5-Me2-2-O)) (5) and NbCl2[ONOO]R(MeCCMe) ([ONOO]R = N(CH2CH2OMe)2(CH2C6H2-3,5-R2-2-O)) (R = tBu, Me) (6), have been synthesized and characterized

  基于四足胺双（酚基）配体NbCl [ONNO] R（MeCCMe）的一系列炔铌配合物（[ONNO] R = N（CH 2 CH 2 NMe 2）2（CH 2 C 6 H 2 -3,5 -R 2 -2-O），R = H，Me）（4）和三足胺酚配体NbCl 2 [ONN] Me（MeCCMe）（[ONN] Me = NMe（CH 2 CH 2 NMe 2）（CH 2 C 6 H 2 -3,5-Me 2 -2-O））（5）和NbCl 2 [ONOO] R（MeCCMe）（[ONOO] R = N（CH 2 CH 2 OMe）2（CH 2 C 6 H 2 -3,5-R 2 -2-O））（R = t Bu，Me）（6），已经通过光谱学和X射线研究合成并表征。对于配合物4和5，已经获得，分离并充分表征了炔烃位置不同的两个异构体。炔配体是反式至侧臂的NMe 2基团或三脚架的氮原子。4和的甲基衍生物参照图5，已经分别合成了NbMe
• Fernandez-Baeza, Juan; Jalon, Felix A.; Otero, Antonio, Journal of the Chemical Society, Dalton Transactions, 1998, # 5, p. 769 - 773
  作者：Fernandez-Baeza, Juan、Jalon, Felix A.、Otero, Antonio、Rodrigo-Blanco, Ma. Esther、Etienne, Michel

  DOI：——

  日期：——