tetrachlorobis(tetrahydrofuran)tin(IV) | 17362-82-2

• 分子结构分类: 有机化合物 - 有机杂环化合物 - 氧唑烯
• 英文名称: tetrachlorobis(tetrahydrofuran)tin(IV)
• 英文别名: SnCl4 * 2 tetrahydrofuran；oxolane;tetrachlorostannane
• CAS: 17362-82-2；216692-33-0；40802-57-1
• 化学式: C₈H₁₆Cl₄O₂Sn
• 分子量: 404.736
• InChiKey: JGJRWNDHBHWJRC-UHFFFAOYSA-J

计算性质

• 辛醇/水分配系数(LogP)：
  3.97
• 重原子数：
  15
• 可旋转键数：
  0
• 环数：
  2.0
• sp3杂化的碳原子比例：
  1.0
• 拓扑面积：
  18.5
• 氢给体数：
  0
• 氢受体数：
  2

反应信息

• 作为反应物：
  描述：

  四氢呋喃氯化钛 、 tetrachlorobis(tetrahydrofuran)tin(IV) 以 四氢呋喃 为溶剂， 以80%的产率得到trans-dichlorotetrakis(tetrahydrofuran)titanate(III) pentachloro(tetrahydrofuran)stannate(IV)
  参考文献：
  名称：

  Interaction of titanium and tin chlorides in tetrahydrofuran. The X-ray crystal structure of [trans-TiCl2(THF)4]+[SnCl5(THF)]−

  摘要：

  DOI：

  10.1016/s0277-5387(00)83888-7
• 作为产物：
  描述：

  四氯化锡 在 四氢呋喃 作用下， 以 四氢呋喃 为溶剂， 生成 tetrachlorobis(tetrahydrofuran)tin(IV)
  参考文献：
  名称：

  通过二苯基硅烷和氯化锡（II）还原氯化钼（V）和氯化钼（IV）的高收率路线，生成钼（III）化合物

  摘要：

  MoCl 4（thf）2已用SnCl 2在化学计量上还原，形成MoCl 3（thf）3并伴有SnCl 4（thf）2的形成。在另一种程序中，MoCl 5根据以下方程式与二苯基硅烷直接反应，根据反应的化学计量，可单步获得高收率的MoCl 4（thf）2或MoCl 3（thf）3 > 85％）合成。MoCl 5 + x Ph 2 SiH 2 →MoCl 5-x（thf）1 + x + x Ph 2 SiHCI + x / 2H 2（x = 1或2）

  DOI：

  10.1016/s0277-5387(00)80226-0
• 作为试剂：
  描述：

  在 tetrachlorobis(tetrahydrofuran)tin(IV) 作用下， 以 甲苯 为溶剂， 以53%的产率得到
  参考文献：
  名称：

  The Porphyrinogen−Porphodimethene Relationship Leading to Novel Synthetic Methodologies Focused on the Modification and Functionalization of the Porphyrinogen and Porphodimethene Skeletons

  摘要：

  The general synthetic methods presented in this paper make available, on a preparative scale, unprecedented porphyrinogen-derived skeletons, including their functionalization at the meso positions. The stepwise dealkylation of meso-octaalkylporphyrinogen R8N4H4 [R = Et, 1; R = Bu-n, 2] was chemically, mechanistically, and structurally followed until the formation of porphomethene and porphodimethene derivatives 5-13, obtained with a sequential use of SnCl4. In particular, the porphodimethene derivative [(Et6N4)SnCl2], 9, was reductively transmetalated using Li metal to Et6N4Li2. 14, subsequently hydrolyzed to Et6N4H2, 15. The porphodimethene-nickel complex [(Et6N4)Ni], 16, was used for studying the reactivity and the ligand modification of the porphodimethene skeleton. The reactivity of 16 toward nucleophiles led to otherwise inaccessible meso-substituted-meso-functionalized porphyrinogens [(Et6N4R2)NiLi2], [R = H, 18; R = Bu-n, 19; R = CH2CN, 20], thus exemplifying a general methodology to meso-functionalized porphyrinogens. In addition, when [NMe2](-) was used as the nucleophile, 16 was converted into mono- and bis-vinylideneporphyrinogen derivatives [{Et-4(=CHMe)N-4}NiLi] 21, and [{Et-5(=CHMe)(2)N-4}NiLi2], 22, through the intermediacy of meso-(dimethylamino)-porphyrinogens undergoing an alpha-II elimination from the meso positions. Such intermediates were isolated and characterized in the stepwise reaction of 14 with LiNMe2 leading to [{Et-6(NMe2)(2)N-4}Li-4], 23, and [{Et-5(NMe2)(=CHMe)N-4}Li-4], 25. Both compounds, as a function of the reaction solvent, undergo the thermal elimination of HNMe2 with the formation of [{Et-4(=CHMe)(2)N-4}Li-4], 24, which is then protonated to [{Et-4(=CHMe)(2)N-4}H-4], 27. Transmetalation from 23 to 24 can be used as the methodology for the synthesis of a remarkable variety of meso-substituted and functionalized porphyrinogen complexes. The deprotonation of 16 is reversible, therefore 22 and 23 can be protonated back to their starting materials. We took advantage of the nucleophilicity of the vinylidene carbon in 21 and 22 fur establishing a general synthetic method to produce meso-functionalized porphodimethenes. This approach was exemplified with the alkylation and the benzoylation of 22 and 21 leading to [{(E4Pr2N4)-N-i)Ni], 28, [Et-4{CH(Me)(PhCO)}(2)N4Ni], 29, and [Et-5{CH(Me)(PhCO)}N4Ni], 30, respectively. Complex 21 displays a bifunctional behavior, as shown by the formation of 30, whereas in the reaction with LiBu, led to [{Et-5(Bu-n)(=CHMe)N-4}NiLi2], 31.

  DOI：

  10.1021/ja000253s

文献信息

• Intramolecular Donor-Assisted Cyclization of Organotin Compounds
  作者：Michael Mehring、Christian Löw、Markus Schürmann、Klaus Jurkschat

  DOI：10.1002/(sici)1099-0682(199905)1999:5<887::aid-ejic887>3.0.co;2-2

  日期：1999.5

  Furthermore, the synthesis of [1(Sn),3(P)-Ph2SnOP(O)(OH)-5-tert-Bu-7-P(O)(OH)2]C6H2 (13) is described. Reaction of 8 with an excess of Me3SiBr leads to the unexpected formation of 2-[P(O)(OEt)(OSiMe3)]-4-tert-Bu-6-[P(O)(OEt)2]C6H2}SnPhBr2 (9) as a result of an O–Sn bond cleavage initiated by Me3SiBr and subsequent reaction of the intermediate with further Me3SiBr under Sn–C bond cleavage. The high donor

  通过从有机锡卤化物开始的取代反应合成了含有单阴离子 O,C,O 配位配体 4-tert-Bu-2,6-[P(O)(OEt)2]2C6H2}- 的新型分子内配位有机锡化合物. 鉴于分子内配位化合物 4-tert-Bu-2,6-[P(O)(OEt)2]2C6H2}SnR2R' (2, R = Ph, R' = CH2SiMe3; 3, R = R' = Ph; 6, R = R' = Cl)，阳离子锡物种被认为是形成杂环化合物 [1(Sn),3(P)-Ph2SnOP(O)(OEt )-5-tert-Bu-7-P(O)(OEt)2]C6H2 (8), [1(Sn), 3(P)-Ph(Me3SiCH2)SnOP(O)(OEt)-5-tert -Bu-7-P(O)(OEt)2]C6H2 (15) 和 [1(Sn),3(P)-Cl2SnOP(O)(OEt)-5-tert-Bu-7-P( O)(OEt)]C6H2}2
• Synthesis of (^tBu₃SiNH)₂ClW⋮WCl(NHSi^tBu₃)₂ and Its Degradation via NH Bond Activation
  作者：Stephen M. Holmes、Daniel F. Schafer、Peter T. Wolczanski、Emil B. Lobkovsky

  DOI：10.1021/ja010957h

  日期：2001.10.31

  NaW2Cl7(THF)5 with 4 equiv of (t)Bu3SiNHLi afforded the C2 W(III) dimer [((t)Bu3SiNH)2WCl]2 (1, d(W triple bond W) = 2.337(2) A), which is a rare, primary amide M2X4Y2 species. Its degradation provided evidence of NH bond activation by the ditungsten bond. Addition of 2 equiv of (t)Bu3SiNHLi or TlOSi(t)Bu3 to 1 yielded H2 and hydride ((t)Bu3SiN)2((t)Bu3SiNH)WH (2, d(WH) = 1.67(3) A) or ((t)Bu3SiN)2((t)Bu3SiO)WH

  用 4 当量的 (t)Bu3SiNHLi 处理 NaW2Cl7(THF)5 得到 C2 W(III) 二聚体 [((t)Bu3SiNH)2WCl]2 (1, d(W 三键 W) = 2.337(2) A) ，这是一种罕见的伯酰胺 M2X4Y2 物种。它的降解提供了二钨键激活 NH 键的证据。将 2 当量的 (t)Bu3SiNHLi 或 TlOSi(t)Bu3 添加到 1 生成 H2 和氢化物 ((t)Bu3SiN)2((t)Bu3SiNH)WH (2, d(WH) = 1.67(3) A) 或((t)Bu3SiN)2((t)Bu3SiO)WH (3)。1 in py 的热解 (60 摄氏度, 16 小时) 得到 ((t)Bu3SiN)2WHCl(py) (4-py, 40-50%), ((t)Bu3SiN)2WCl2(py) (6-py, 10%) 和 ((t)Bu3SiN)2HW(mu-
• Spectroscopic (119Sn and 13C NMR, 119mSn Mössbauer and IR) studies of tin(IV) tetrahalide adducts of cyclic and aromatic ethers, in the solid state and in solution
  作者：Stephen J. Blunden、Diane Searle、Peter J. Smith

  DOI：10.1016/s0020-1693(00)87602-1

  日期：1985.4

  Abstract The interaction of tin(IV) halides (SnCl 4 and SnBr 4 ) with a series of cyclic and aromatic ethers has been studied in the solid state and in solution. Nine solid adducts of composition, SnX 4 ·2(ether) and SnCl 4 ·(ether), were isolated and their structures investigated by 119m Sn Mossbauer and IR spectroscopy. The 1:2 adducts contain an octahedral tin atom geometry, with trans -coordinated

  摘要研究了卤化锡（IV）（SnCl 4和SnBr 4）与一系列环状和芳族醚在固态和溶液中的相互作用。分离出九种固体组成的SnX 4·2（醚）和SnCl 4·（醚）加合物，并通过119m Sn Mossbauer和红外光谱对其结构进行了研究。1：2加合物具有八面体锡原子几何形状，并带有反式配位的醚配体。在SnX 4 /醚系统上的119 Sn和13 C NMR研究表明，在某些情况下，有可能在溶液中形成六配位络合物。比较了各种醚对卤化锡（IV）的相对供体能力。
• Adducts of tin(IV) tetrahalides with neutral lewis bases. I. Vibrational study of the cis-trans isomerism in solution
  作者：S.J. Ruzicka、A.E. Merbach

  DOI：10.1016/s0020-1693(00)94120-3

  日期：1976.1

  Abstract A large number of SnX4·2L and SnX4·L-L tin(IV) tetrahalide adducts were synthesized and analyzed (X = Cl, Br; L = Me2O, Et2O, THF, Me2S, Et2S, THT, Me2Se, MeCN, Me3CCN, Me3CO, HMPA, TMPA; L−L = (MeOCH2−)2). Their cis or trans geometry was determined by infrared and Raman spectroscopy. For the SnCl4·2THT adduct, both isomers could be isolated by changing the solvent polarity. The existence

  摘要合成并分析了大量的SnX4·2L和SnX4·LL四卤化锡（IV）加合物（X = Cl，Br; L = Me2O，Et2O，THF，Me2S，Et2S，THT，Me2Se，MeCN，Me3CCN，Me3CO ，HMPA，TMPA； L =（MeOCH2-）2）。它们的顺式或反式几何结构通过红外和拉曼光谱法测定。对于SnCl4·2THT加合物，可以通过改变溶剂极性来分离两种异构体。对于大多数加合物，通过拉曼测量已证明溶液中存在顺式-反式平衡。这种平衡在很大程度上取决于溶剂的极性，顺式异构体在高极性介质中是有利的。使用威尔逊FG矩阵的简化模型，确定Sn-X力常数，并推导以下序列以得出SnX4·2L中锡-配体键的强度：Me2Se> Me2S〜THT〜Et2S>
• Molecular Structures of two Cyclic Bis(amino)tin Dichlorides and their NMR Spectroscopic Characterization in Solution. — The First 1, 3, 2‐Diazastanna‐[3]ferrocenophane
  作者：Bernd Wrackmeyer、Wolfgang Milius、Heidi E. Maisel、Hendrik Vollrath、Max Herberhold

  DOI：10.1002/zaac.200300026

  日期：2003.7

  2, 2‐Dichloro‐1, 3‐bis(trimethylsilyl)‐1, 3, 2‐diazastanna‐[3]ferrocenophane (6) was prepared for the first time, characterized in solution by ¹H, ¹³C, ¹⁵N, ²⁹Si and ¹¹⁹Sn NMR spectroscopy, and in the solid state by X‐ray structural analysis. The cyclopentadienyl rings are almost parallel and the atoms Fe, C(1), N, Sn form a plane. For comparison, the synthesis of another cyclic bis(amino)tin dichloride (2) with the 1, 3, 2, 4, 5‐diazastannadisila‐cyclopentane ring was repeated, and the molecular structure of 2 was determined by X‐ray crystallography. The five‐membered heterocycle is almost planar, and most structural parameters of 2 compare favorably with those of 6. In contrast to the ferrocenophane 6, the heterocycle 2 is well soluble and stable in solution. Thus, it proved possible to carry out a number of non‐routine 1D and 2D heteronuclear double resonance experiments for 2 in order to determine the absolute signs of the coupling constants ¹J(¹¹⁹Sn, ¹⁵N) (> 0), ²J(¹¹⁹Sn, ²⁹Si) (> 0), ^{2, 3}J(¹¹⁹Sn, ¹³C) (n = 2; > 0; n = 3: < 0) and ⁴J(¹¹⁹Sn, ¹H) (¹¹⁹Sn‐N‐C‐C‐¹H: < 0; ¹¹⁹Sn‐N‐Si‐C‐¹H: > 0) in this type of compound for the first time.

  摘要 首次制备了 2，2-二氯-1，3-双（三甲基硅基）-1，3，2-二氮杂-[3]二茂铁（6），并通过 1H、13C、15N、29Si 和 119Sn NMR 光谱分析和 X 射线结构分析确定了其溶液特征和固态特征。环戊二烯环几乎平行，Fe、C(1)、N、Sn 原子形成一个平面。为了进行比较，我们重复合成了另一种具有 1，3，2，4，5-二氮杂锡二甲环戊二烯环的环状双（氨基）二氯化锡（2），并通过 X 射线晶体学确定了 2 的分子结构。与二茂铁 6 相比，杂环 2 在溶液中溶解性好且稳定。因此，事实证明可以对 2 进行一系列非例行的一维和二维异核双共振实验，以确定耦合常数 1J（119Sn，15N）（> 0）、2J（119Sn，29Si）（> 0）、2、3J（119Sn，13C）（n = 2；> 0；n = 3：0) 和 4J(119Sn, 1H) (119Sn-N-C-C-1H: < 0; 119Sn-N-Si-C-1H: >0)。