Bis<6-O,6-O'-(1,2:3,4-diisopropylidene-α-D-galactopyranosyl)thiophosphoryl> disulfide

• 分子结构分类: 有机化合物 - 有机杂环化合物 - 二氧吡喃
• 英文名称: Bis<6-O,6-O'-(1,2:3,4-diisopropylidene-α-D-galactopyranosyl)thiophosphoryl> disulfide
• 英文别名: bis[O,O'-bis(1,2;3,4-di-O-isopropylidene-α-D-galactopyranos-6-yl)dithiophosphoryl] disulfide；bis[6-O,6'-O-(1,2:3,4-diisopropylidene-α-D-galactopyranosyl)thiophosphoryl] disulfide；bis[6-O,6-O'-(1,2:3,4-diisopropylidene-α-D-galactopyranosyl)thiophosphoryl] disulfide；[bis[[(1S,2R,6R,8R,9S)-4,4,11,11-tetramethyl-3,5,7,10,12-pentaoxatricyclo[7.3.0.02,6]dodecan-8-yl]methoxy]phosphinothioyldisulfanyl]-sulfanylidene-bis[[(1S,2R,6R,8R,9S)-4,4,11,11-tetramethyl-3,5,7,10,12-pentaoxatricyclo[7.3.0.02,6]dodecan-8-yl]methoxy]-lambda5-phosphane；[bis[[(1S,2R,6R,8R,9S)-4,4,11,11-tetramethyl-3,5,7,10,12-pentaoxatricyclo[7.3.0.02,6]dodecan-8-yl]methoxy]phosphinothioyldisulfanyl]-sulfanylidene-bis[[(1S,2R,6R,8R,9S)-4,4,11,11-tetramethyl-3,5,7,10,12-pentaoxatricyclo[7.3.0.02,6]dodecan-8-yl]methoxy]-λ5-phosphane
• 化学式: C₄₈H₇₆O₂₄P₂S₄
• 分子量: 1227.33
• InChiKey: BVHGOMUHVAEXNH-JRJIBKJTSA-N

计算性质

• 辛醇/水分配系数(LogP)：
  5
• 重原子数：
  78
• 可旋转键数：
  15
• 环数：
  12.0
• sp3杂化的碳原子比例：
  1.0
• 拓扑面积：
  336
• 氢给体数：
  0
• 氢受体数：
  28

反应信息

• 作为产物：
  描述：

  triethylamine O,O'-bis(1,2;3,4-di-O-isopropylidene-α-D-galactopyranos-6-yl)dithiophosphoric acid salt 在 碘 作用下， 以 水 、 甲苯 为溶剂， 生成 Bis<6-O,6-O'-(1,2:3,4-diisopropylidene-α-D-galactopyranosyl)thiophosphoryl> disulfide
  参考文献：
  名称：

  超分子宿主-客体组合的合成和固态研究：Bis [6- O，6- O '-（1,2：3,4-二异亚丙基-α-d-吡喃半乳糖基）硫代磷酰基]双硫属化物

  摘要：

  提出了一种补充方法，用于研究由对称和不对称二硫代双氰化物形成的复杂固体材料的结构细节，该方法同时使用X射线衍射（XRD）和固态NMR（SS NMR）。新的诊断技术允许在晶格中的客体迁移过程中，可逆的晶体空间群变化和主体几何形状的非常细微的变形得以遵循。可以合成双[6- O，6- O '-（1,2：3,4-二异亚丙基-α - d-吡喃半乳糖基）]硫代磷酰基亚硒基硫化物，它是轮轴主体（WAAH）分子的代表通过研磨和缓慢加热二硫化物1和二硒化物2而形成固态。二硫化物的全面表征1在固相中已经报道（有机化学杂志。 1995年，60，2549）。在当前的工作中，介绍了同结构二硒化物底物2的合成以及XRD和SS NMR研究。采用31 P交叉极化魔角旋转实验跟踪硒硒烯3的合成进展在固态。结论是，在液体和粉末状固体中，硒烯基硫化物与二硫化物和二硒化物以1：1：1的比例平衡存在。从不同溶剂中结晶出来的同构二卤

  DOI：

  10.1021/jo8002997

文献信息

• Studies of Solvate and Inclusion Complexes of Bis[6-O,6-O'-(1,2:3,4-Diisopropylidene-.alpha.-D-galactopyranosyl)- thiophosphoryl] Disulfide in the Solid State by NMR and X-ray Methods
  作者：Marek J. Potrzebowski、Jaroslaw Blaszczyk、Michal W. Wieczorek

  DOI：10.1021/jo00113a039

  日期：1995.4

  P-31 CP/MAS spectroscopy was used to recognize different crystallographic forms of bis[6-O,6-O'-(1,2:3,4-diisopropylidene-alpha-D-galactopyranosyl) thiophosphoryl] disulfide, From analysis of P-31 chemical shift parameters, anisotropy Delta delta, and asymmetry eta it was concluded that each polymorph under investigation has anti-anti geometry of S=P-S-S-P=S skeleton and S=P-S angles in the range 105-107 degrees. The P=S and P-S distances for appropriate polymorphs are almost identical. H-2 CP/MAS showed that solvent molecules are included in the crystallographic lattice. From line shape analysis of Pake doublets the fast molecular motion of benzene-d(6) with correlation time tau(c) < 10(-7) was established. Three different crystallographic forms of disulfide 1a-c determined by XRD belong to different crystallographic systems and space groups. The differences are connected with kind and amount of solvent used in crystallization. Crystals of 1a are orthorhombic, P2(1)2(1)2(1), with a = 10.536(4) Angstrom, b = 25.067(4) Angstrom, c = 28.021(5) Angstrom, V = 7401(4) Angstrom(3), Z = 4, D-c = 1.249(2)g cm(-3). Refinement using 2693 observed reflections for 811 parameters gives R = 0.067. The asymmetric part ofthe unit cell contains one molecule of 1 with one molecule of benzene and one molecule of hexane. Crystals of 1b are monoclinic, space group P2(1), with a = 10.4293(8) , b = 28.206(2) Angstrom, c = 12.105(1) Angstrom, beta = 90.696(8)degrees, V = 3560.6(7) Angstrom(3), Z = 2, D-c = 1.367(2)8 cm(-3). Refinement using 6504 observedreaections for 775 parameters gives R = 0.060. The asymmetric part of the unit cell contains one molecule of 1 with two molecules of chloroform, Crystals of Ic are trigonal, space group P3(2), with a = b = 11.861(1) Angstrom, c = 44.679(3) Angstrom, V = 5443(3) Angstrom(3), Z = 3, D-c = 1.266(2) g cm(-3). Refinement using 3191 observed reflections for 811 parameters gives R = 0.040. The asymmetric part of the unit cei contains one molecule of 1 with two molecules of benzene. Variable temperature P-31 CP/MAS and; H-2 CP/MAS studies revealed that crystals of la and Ic form inclusion complexes with solvent which are unstable and undergo a phase transition below the melting point.
• Synthesis and Solid-State Study of Supramolecular Host−Guest Assemblies: Bis[6-<i>O</i>,6-<i>O</i>′-(1,2:3,4-diisopropylidene-α-<scp>d</scp>-galactopyranosyl)thiophosphoryl] Dichalcogenides
  作者：Marek J. Potrzebowski、Wojciech M. Potrzebowski、Agata Jeziorna、Wlodzimierz Ciesielski、Jarosław Gajda、Grzegorz D. Bujacz、Maksymilian Chruszcz、Wladek Minor

  DOI：10.1021/jo8002997

  日期：2008.6.1

  for studying structural details of complex solid materials formed by symmetrical and unsymmetrical dichalcogenides, which employs both X-ray diffraction (XRD) and solid-state NMR (SS NMR), is presented. The new diagnostic technique allows reversible crystallographic space group change and very subtle distortion of host geometry to be followed during guest migration in the crystal lattice. Bis[6-O,6-O′-(1

  提出了一种补充方法，用于研究由对称和不对称二硫代双氰化物形成的复杂固体材料的结构细节，该方法同时使用X射线衍射（XRD）和固态NMR（SS NMR）。新的诊断技术允许在晶格中的客体迁移过程中，可逆的晶体空间群变化和主体几何形状的非常细微的变形得以遵循。可以合成双[6- O，6- O '-（1,2：3,4-二异亚丙基-α - d-吡喃半乳糖基）]硫代磷酰基亚硒基硫化物，它是轮轴主体（WAAH）分子的代表通过研磨和缓慢加热二硫化物1和二硒化物2而形成固态。二硫化物的全面表征1在固相中已经报道（有机化学杂志。 1995年，60，2549）。在当前的工作中，介绍了同结构二硒化物底物2的合成以及XRD和SS NMR研究。采用31 P交叉极化魔角旋转实验跟踪硒硒烯3的合成进展在固态。结论是，在液体和粉末状固体中，硒烯基硫化物与二硫化物和二硒化物以1：1：1的比例平衡存在。从不同溶剂中结晶出来的同构二卤