4,4′-二苯基-2,2′-双噻唑-5,5′-二磺酸二钠的合成

以二硫代乙二酰胺、ω一溴代苯乙酮为起始原料,合成了4,4′-二苯基-2,2′-双噻唑.m.p.216.9℃-217.1℃,收率57.5%.IR,νmax(cm-1):3111(Ar-H),3060(Ph-H),1597,1558,1541,1508,1474,1443(苯环骨架,噻唑环骨架振动),939,742,692(苯环单取代).后经磺化,中和生成4,4′-二苯基-2,2′-双噻唑-5,5′-二磺酸二钠.m.p.>300℃,收率44%.IR,νmax(cm-1):1236,1184,1126,1047(R-SO3-).1H NMR,δ(ppm):7.63,7.56,7.51(苯H).

Crystal and Molecular Structure of 1-Methyl-4-(2-( 3,4-dimethoxyphenyl) vinyl) pyridinium 4-Tolylsulfonate Dihydrate C_(16)H_(18)NO_2^+·C_7H_7SO_3^-·2H_2O

The crystal structure of the title compound C16H18NO2+·C7H7SO3-·2H2O, (C23H29NSO7, Mr=463.53) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system with space group P21/n, a=8.101(1), b=8.958(2), c=33.281(5)?,β= 94.910(1)(, V=2406.3(7)?3, Z=4, Dc=1.279g/cm3, μ=0.176mm-1, F(000)=984, final R=0.0409, and Rw=0.0860 for 4401 independent reflections. The result shows that in the crystal structure of the title compound the planar cations have two configurations with equal occupation ratio and are antiparally packed through π…π interactions. Similar packing energies in A and B are probably the main factor that leads to the disorder structure.

Chiral Phosphine Ligands Derived from Sugars8. Crystal and Molecular Structure of Diphenyl (methyl 4', 6'-O-benzylidene-2'-deoxy-α-D-altropyranoside-2-)phosphine Oxide

The crystal structure of the title compound, C26H27O6P, has been determined by single--crystal X-ray diffraction. The crystal is monoclinic with space groupP21, a=16. 193(l), b=5. 804(1), c=12. 512(2) A, β=93. 187(5)°, V=1174. 13A3, Dc=1. 319 g/cm3, F(000) =492, μ= 13. 52 cm-1, Z= 2, and final R= 0. 042and Rw= 0. 040 for 2349 reflections (I≥3σ(I)). Structure analysis revealed that thepyranose and 4, 6-O-benzylidene ring of the title compound adopts a distorted chair conformation.

Synthesis and Crystal Structure of an Ion- pair Compound: [HL]_2[Ni(CN)_4]·4H_2O (L = 4-(2- Hydroxyphenyl)-1,5, 9-triazacyclododecan-2-one)

An ion-pair compound, [HL]2[Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphenyl)-1,5,9-triazacyclododecan-2-one) in aqueous solution, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.380(1), b = 9.9637(8), c = 17.087(1) ? ?= 105.947(2)? V = 2026.6(3) ?, Rint = 0.0509, Z = 2, Dc = 1.297 g/cm3, C34H56O8N10Ni, Mr = 791.60, F(000) = 844, m(MoKa) = 0.538 mm1, S = 1.030, the final R = 0.0644 and wR = 0.1299 for 2023 observed reflections with I ≥ 2(I). The title compound 1 contains one anion of [Ni(CN)4]2, two cations of [HL]+ and four packing water molecules, which are held together by the NH···O and OH···O hydrogen bonds to form a three- dimensional framework.

X-ray Structure of 1- (3' -Phenyl-4' -morpholinyl-2' 5' - dithiole-1' - ylidene)-3, 4-biscarboethoxy-2-thionaphthalene

The title compound (C28H27NO5S3, Mr= 553. 69) was prepared bythe reaction of a-thiobenzoylthioformmorholine with diethyl acetylene dicarboxylate.The crystal is monoclinic, space group P21/n with a= 9. 160(3), b= 17. 726(3), c=16. 602(3) A ; β= 100. 375(13)°; V=2651. 4(10) A3, Z=4, Dc= 1. 387 g/cm3, μ(MoKa) =0. 319 mm-1, F(000) =1160, R=0. 0428, wR(F2) =0. 0910 for 2438 observed reflections (I>2(I)). X-ray analysis reveals that interatomic distances for C(5)-C(6), C(13)-C(14) and C(21)-C(22) are 1. 331(4), 1. 351(4), 1. 344(4)A respectively, which show that they are normal C=C double bonds. All S-C bondlengths are similar to typical S-C single bonds (1. 75 - 1. 78 A ). The five-membered ring A (C(5) -C(6) -S(2)-C(13) -S(1) ) (Fig. 1) and six-membered ringB (C(14) -C(15) -C(20) -C(21)-C(22)-S(3) ) (Fig. 1) adopt the flat twist conformation. Furthermore, the morpholine ring adopts chair conformtion.

Synthesis and luminescent properties of ternary complex Eu(UVA)_3Phen in nano-TiO_2

By introducing 2-hydroxy-4-methoxy-benzophenone(UVA) and 1,10-phenanthroline(Phen) as the ligands, the ternary rare earth complex of Eu(UVA)3Phen is synthesized, and it is characterized by elemental analysis, mass spectra(MS) and infrared(IR) and ultraviolet(UV) spectroscopy. Results show that the Eu(III) in complex emits strong red luminescence when it is excited by UV light, and it has higher sensitized luminescent efficiency and longer lifetime. The organic-inorganic thin film of complex Eu(UVA)3Phen doped with nano-Ti O2 is prepared, and the nano-Ti O2 is used in the luminescence layer to change the luminescence property of Eu(UVA)3Phen. It is found that there is an efficient energy transfer process between ligands and metal ions. Moreover, in an indium tin oxide(ITO)/poly(N-vinylcar-bazole)(PVK)/Eu(UVA)3Phen/Al device, Eu3+ can be excited by intramolecular ligand-to-metal energy transfer process. The main peak of emission at 613 nm is attributed to 5D0→7F2 transition of the Eu3+, and this process results in the enhanced red emission.

Convergent Strategy to Synthesize (S)-8-(4-((1-(3-Fluoropropyl)-pyrrolidin-3-yl)oxy)phenyl)-7-(4-hydroxyphenyl)-5,6-dihydronaphthalen-2-ol as a Selective Estrogen Receptor Degrader

A more feasibly convergent synthesis of selective estrogen receptor degrading agent(S)-8-(4-((1-(3-fluoropropyl)-pyrrolidin-3-yl)oxy)phenyl)-7-(4-hydroxyphenyl)-5,6-dihydronaphthalen-2-ol was reported,featured with concise work up and absence of regioselectivity dilemma.