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Motoo Shiro

Publications and source records attributed to Motoo Shiro.

At least 19 recordsLinked to original sources

Synthesis, structures, and properties of meso-phosphorylporphyrins: self-organization through P-oxo-zinc coordination.

The synthesis, structures, and optical and electrochemical properties of meso-phosphorylporphyrins are described. The copper-catalyzed carbon-phosphorus cross-coupling reaction of a meso-iodoporphyrin with di-n-butyl phosphite and diphenylphosphane oxide has proved to be an efficient and general method for the synthesis of meso-phosphorylporphyrins. Zinc phosphorylporphyrins thus obtained readily undergo self-organization through P-oxo-Zn coordination to form noncovalently linked, cofacial porphyrin dimers or linear oligomers, which have been characterized by spectroscopic methods and X-ray crystallographic analyses. In toluene, CH(2)Cl(2), and CHCl(3), the zinc phosphorylporphyrins exist mostly as dimers or monomers, depending on their concentrations, the temperature, and the presence of additives. The self-association constants for dimerization in toluene have been determined by UV/Vis absorption titration measurements. The meso-diphenylphosphorylporphyrin dimer displays excitonic coupling of the Soret band with a splitting energy of 940 cm(-1). Fluorescence lifetimes of the zinc phosphorylporphyrins have been found to be affected only slightly by the concentration of the solution, and by the addition of triphenylphosphane oxide, suggesting that the effect of dimerization on their photodynamics in the S(1) state is negligible. On the other hand, the effect of dimerization is clearly reflected in their electrochemical oxidation processes, as the initially produced radical cations are efficiently delocalized over the two porphyrin rings. These findings demonstrate the potential utility of meso-phosphorylporphyrins as new models for the special pair in photosynthesis and as new building blocks for porphyrin-based supramolecular materials.

Crystallography, X-Ray↗

Key role of the Lewis base position in asymmetric bifunctional catalysis: design and evaluation of a new ligand for chiral polymetallic catalysts.

New chiral ligands for asymmetric polymetallic catalysts were designed on the basis of the assumption that the higher-order assembly structure is stabilized by modifying the modular unit. The designed ligands 6 and 7 contained a scaffolding cyclohexane ring with a Lewis base phosphine oxide directly attached to the scaffold. A module in the polymetallic complex contains two metals per ligand, and a stable 6-, 5-, 5-membered fused chelation ring system should be generated. Synthesis of these ligands is simple and high yielding, using a catalytic dynamic kinetic resolution promoted by the Trost catalyst as a key step. Ligand function was assessed in a catalytic asymmetric ring-opening reaction of meso-aziridines with TMSCN, a useful reaction for the synthesis of optically active beta-amino acids. The Gd complex generated from Gd(OiPr)3 and the ligand was a highly active and enantioselective catalyst in this reaction. Enantioselectivity was reversed compared to the previously reported d-glucose-derived catalyst containing the same chirality of the individual module. ESI-MS analysis and X-ray crystallographic studies indicate that the assembly state of the modules in the polymetallic catalysts differs depending on the chiral ligand. The difference in the higher-order structure stems from a subtle change (one carbon) in the position of the Lewis base relative to the Gd metal. The change in the higher-order structure of the polymetallic complex led to a dramatic reversal of the enantioselectivity and increased catalyst activity.

Aziridines↗

A new fluorescent probe for zinc(II): an 8-hydroxy-5-N,N-dimethylaminosulfonylquinoline-pendant 1,4,7,10-tetraazacyclododecane.

A new fluorescent probe for Zn2+, namely, 8-hydroxy-5-N,N-dimethylaminosulfonylquinolin-2-ylmethyl-pendant cyclen (L8), was designed and synthesized (cyclen=1,4,7,10-tetraazacyclododecane). By potentiometric pH, 1H NMR, and UV spectroscopic titrations, the deprotonation constants pKa1-pKa6 of L(8)4 HCl were determined to be <2, <2, <2 (for amino groups of the cyclen and quinoline moieties), 7.19+/-0.05 (for 8-OH of the quinoline moiety), 10.10+/-0.05, and 11.49+/-0.05, respectively, at 25 degrees C with I=0.1 (NaNO3). The results of 1H NMR, potentiometric pH, and UV titrations, as well as single-crystal X-ray diffraction analysis, showed that L8 and Zn2+ form a 1:1 complex [Zn(H-1L8)], in which the 8-OH group of the quinoline ring of L8 is deprotonated and coordinates to Zn2+, in aqueous solution at neutral pH. On addition of one equivalent of Zn2+ and Cd2+, the fluorescence emission of L8 (5 microM) at 512 nm in aqueous solution at pH 7.4 [10 mM HEPES with I=0.1 (NaNO3)] and 25 degrees C increased by factors of 17 and 43, respectively. We found that the cyclen moiety has the unique property of quenching the fluorescence emission of the quinolinol moiety when not complexed with metal cations, but enhancing emission when complexed with Zn2+ or Cd2+. In addition, the Zn2+-L8 complex [Zn(H-1L8)] is much more thermodynamically and kinetically stable (Kd{Zn(H-1L8)}=[Zn2+]free[L8]free/[Zn(H-1L8)]=8 fM at pH 7.4) than the Zn2+ complexes of our previous Zn2+ fluorophores ([Zn(H-1L2)] and [Zn(L3)]). Furthermore, formation of [Zn(H-1L8)] is much faster than those of [Zn(H-1L2)] and [Zn(L3)]. The staining of early-stage apoptotic cells with L8 is also described.

Amines↗

Total syntheses of zaragozic acids A and C by a carbonyl ylide cycloaddition strategy.

A carbonyl ylide cycloaddition approach to the squalene synthase inhibitors zaragozic acids A and C is described. The carbonyl ylide precursor 8 was synthesized starting from di-tert-butyl D-tartrate (47) via an eleven-step sequence involving the regioselective reduction of the mono-MPM (MPM=4-methoxybenzyl) ether 48 with LiBH4 and the diastereoselective addition of sodium tert-butyl diazoacetate to alpha-keto ester 10. The reaction of alpha-diazo ester 8 with 3-butyn-2-one (40) in the presence of a catalytic amount of [Rh2(OAc)4] gave the desired cycloadduct 59 as a single diastereomer. The dihydroxylation of enone 59 followed by sequential transformations permitted the construction of the fully functionalized 2,8-dioxabicyclo[3.2.1]octane core 5. Alkene 79 derived from 5 serves as a common precursor to zaragozic acids A (1) and C (2), since the elongation of the C1 alkyl side chain can be attained by olefin cross-metathesis, especially under the influence of Blechert's catalyst (85).

Alkenes↗

Stereochemical course in water addition during LUP1-catalyzed triterpene cyclization.

Arabidopsis thaliana LUP1 (At1g78970) catalyzes the cyclization of oxidosqualene into lupeol and 3beta,20-dihydroxylupane (lupanediol). The stereochemical course of water addition to the lupanyl cation was studied. The X-ray crystal structure of lupanylepoxide 3,5-dinitrobenzoate established the configuration of epoxide as 20S. LiAlD4 reduction of the epoxide enabled the chemical shift assignment of prochiral methyl groups at C20 of lupanediol. Correlation of these methyl groups with biosynthetic lupanediol from [1,2-(13)C(2)] acetate established the stereochemical course of water addition. [reaction: see text].

Arabidopsis Proteins↗

Synthesis and antibacterial activities of new quinolone derivatives utilizing 1-azabicyclo[1.1.0]butane.

The ring-opening reactions of 1-azabicyclo[1.1.0]butane 3 with thiols 6a-f gave 3-sulfenylazetidine derivatives 7a-f in 50-92% yields. Treatment of 3 with aromatic amines 11a-e and dibenzylamine 11f in the presence of Mg(ClO(4))(2) afforded the corresponding 3-aminoazetidine derivatives 12a-f in 24-53% yields. These azetidine derivatives were introduced into the C7 position of a quinolone nucleus 8 to afford the corresponding fluoroquinolones 9a-f and 13a-f in 21-83% yields. Some of them exhibited superior antibacterial activity against quinolone-susceptible MRSA in comparison with clinically used fluoroquinolones, such as levofloxacin, ciprofloxacin, and gatifloxacin.

Anti-Bacterial Agents↗

Synthesis and structure of new water-soluble and stable tantalum compound: ammonium tetralactatodiperoxo-mu-oxo-ditantalate(V).

The stable water-soluble tantalum complex with lactic acid (ammonium tetralactatodiperoxo-mu-oxo-ditantalate(V)), (NH4)4[Ta2(C3H4O3)4(O2)2O].3H2O, was prepared in the crystalline form. According to the single-crystal X-ray diffraction data, this compound forms a monoclinic cell with a = 13.85(2) A, b = 9.06(1) A, c = 12.32(2) A, and beta = 116.30 degrees , space group C2 (No. 2), and has Z = 2 molecules per unit cell. The solid-state 13C NMR data and low flack parameter are consistent with the determined structure. Appearance of the same vibration modes in Raman and IR spectra supports the choice of the space group without inversion symmetry. The solution of the tantalum complex was successfully applied for the synthesis of two photocatalytic materials, NaTaO3 and Sr2Ta2O7.

Journal Article↗

Highly stereoselective asymmetric Pummerer reactions that incorporate intermolecular and intramolecular nonbonded S...O interactions.

New chiral sulfoxides (R(S),S)-3, (S(S),S)-3, (R(S),S)-4, and (S(S),S)-4 and known chiral sulfoxides (R(S))-5, (R(S))-6, and (R(S))-7 were synthesized, and the stereochemistry of the new sulfoxides (R(S),S)-3 and (R(S),S)-4 was determined by X-ray crystallographic analysis. In their crystallographic structures, the intramolecular nonbonded S...O close contacts were recognized. Analyses of several sulfoxide complexes including rac-11 with N,N-dimethylacetamide (DMAC) or N-methyl-2-pyrrolidone (NMP) in a MeOH solution utilizing cold-spray ionization mass spectrometry provided, for the first time, direct information for intermolecular nonbonded S...O interactions between sulfoxides and amide (or lactam) in a solution. Highly diastereoselective and enantioselective Pummerer reactions based on the concept of intermolecular and intramolecular nonbonded S...O interactions were performed by treatment of several chiral sulfoxides (R(S), S)-3, (S(S), S)-3, (R(S), S)-4, (S(S), S)-4, (R(S))-5, (R(S))-6, and (R(S))-7 with acetic anhydride and trimethylsilyl triflate (TMSOTf) in DMAC, NMP, N,N-dimethylformamide, and N-formylpiperidine. Mechanistic studies on these facile stereoselective Pummerer reactions revealed the necessity for the amide/TMSOTf complex, such as 26 or 27, to be an efficient activation reagent for Ac(2)O and a trapping reagent for the released acetate ion, and that DMAC and NMP had a positive effect on this highly stereoselective chiral transfer reaction.

Journal Article↗

Synthesis and characterization of bromonium ylides and their unusual ligand transfer reactions with N-heterocycles.

Stable aliphatic bromonium ylides (RfSO2)2C--Br+C6H4-p-CF3 (Rf = CF3, CF3(CF2)3) have been synthesized and structurally characterized for the first time. X-ray crystallographic analyses indicated a ylide structure with an sp2 hybridization of the ylide carbanions and with little double-bond character for the ylidic bond. The bromonium ylides selectively undergo transfer of the aryl group to nitrogen heterocycles, such as pyridines, yielding N-arylpyridinium salts. This is in a marked contrast to the reaction of the iodonium ylides, which produces pyridinium ylides through transylidations.

Journal Article↗

(1Z,2Z)-1,2-Bis(3-methyl-2,3-dihydro-1,3-benzothiazol-2-ylidene)hydrazine.

The title compound, C16H14N4S2, crystallizes in symmetry group C2. The molecule is planar with C2h symmetry, with the inversion centre at the mid-point of the hydrazine N-N bond, and it has an N-N s-trans conformation and a Z,Z configuration. The particular crystal examined was a racemic twin, as suggested by the Flack parameter of 0.41 (2) [Flack (1983). Acta Cryst. A39, 876-881].

Benzothiazoles↗

Self-assembly of multinuclear complexes with enantiomerically pure chiral binaphthoxy imine ligands: effect of the alkyl spacer connecting two binaphthyl units on the metal binding.

Metal complexing behavior of enantiomerically pure alpha,omega-diiminoalkanes possessing the two terminal binaphthyl units (L1 and L2) was studied. The ligands L1 and L2 were prepared by the reaction of optically pure 2'-butoxy-3-formyl-2-hydroxy-1,1'-binaphthyl with propane and pentane diamines. Reactions of L1 and L2 with equimolar amount of Cu(OAc)2 afforded quantitatively multinuclear complexes 1. The structure of 1 was confirmed by MALDI-TOF MS spectroscopy, X-ray single-crystal-structure analysis, and UV/vis and CD spectroscopic analyses. The reaction of L1 having a 1,3-propanediyl spacer resulted in the formation of a self-assembled product, which was assigned as enantiopure trinuclear circular helicate 1a, while the ligand having a 1,5-pentanediyl spacer L2 gave a different self-assembled product, dinuclear side-by-side complex 1b. The circular dichroism (CD) spectrum of 1a in solution showed intense Cotton effects in both the pi-pi* transition of the naphthalene units and the LMCT region of the N,O-chelate moieties. The CD spectrum of 1b was completely different from that of 1a; in particular the Cotton effects in the LMCT region were very weak, contrary to those of 1a. These results suggest that 1a retains some chirality induced on the N,O-chelating moieties even in solution, while the induced chirality on the N,O-chelating moieties in 1b is not very significant, being consistent with the consequences of the X-ray single-crystal-structure studies.

Journal Article↗

Expeditious syntheses of conjugated allenyl esters and oxazoles through a cascade reaction of alpha-alkynyl malonates under alkaline conditions.

Diethyl alpha-alkynyl-alpha-methoxymalonates (2a--e) were smoothly hydrolyzed and then decarboxylated under alkaline conditions employing 1 N KOH in EtOH to give conjugated allenyl esters (6a--e) in high yields, and similar alkaline treatment of diethyl alpha-alkynyl-alpha-acetylaminomalonates (5a, b, d, e) furnished unexpectedly the oxazoles (7a, b, d, e) having three substituent groups in excellent yields.

Alkalies↗

Dioxo-molybdenum(VI) and mono-oxo-molybdenum(IV) complexes supported by new aliphatic dithiolene ligands: new models with weakened Mo=O bond characters for the arsenite oxidase active site.

The cis-dioxo-molybdenum(VI) complexes, [MoO2(L(H))2]2- (1b), [MoO2(L(S))(2)]2- (2b), and [MoO2(L(O))2]2- (3b) (L(H) = cyclohexene-1,2-dithiolate, L(S) = 2,3-dihydro-2H-thiopyran-4,5-dithiolate, and L(O) = 2,3-dihydro-2H-pyran-4,5-dithiolate), with new aliphatic dithiolene ligands were prepared and investigated by infrared (IR) and UV-vis spectroscopic and electrochemical methods. The mono-oxo-molybdenum(IV) complexes, [MoO(L(H))2]2- (1a), [MoO(L(S))2]2- (2a), and [MoO(L(O))2]2- (3a), were further characterized by X-ray crystal structural determinations. The IR and resonance Raman spectroscopic studies suggested that these cis-dioxo molybdenum(VI) complexes (1b-3b) had weaker Mo=O bonds than the common Mo(VI)O2 complexes. Complexes 1b-3b also exhibited strong absorption bands in the visible regions assigned as charge-transfer bands from the dithiolene ligands to the cis-MoO2 cores. Because the oxygen atoms of the cis-Mo(VI)O2 cores are relatively nucleophilic, these complexes were unstable in protic solvents and protonation might occur to produce Mo(VI)O(OH), as observed with the oxidized state of arsenite oxidase.

Binding Sites↗

Effects of complexation with 18-crown-6 on the hypernucleofugality of phenyl-lambda3-iodanyl groups. Synthesis of vinyl-lambda3-iodane.18-crown-6 complex.

[structure: see text] 4-tert-Butyl-1-cyclohexenyl(phenyl)(tetrafluoroborato)-lambda(3)-iodane forms a discrete supramolecular complex by the reaction with 18-crown-6. Solvolysis of the cyclohexenyl-lambda(3)-iodane in the presence of 18-crown-6 indicates that the complexation with 18-crown-6 tends to decrease the leaving group ability of hypervalent phenyl-lambda(3)-iodanyl groups.

Journal Article↗

A luminescence sensor of inositol 1,4,5-triphosphate and its model compound by ruthenium-templated assembly of a bis(Zn2+-cyclen) complex having a 2,2'-bipyridyl linker (cyclen = 1,4,7,10-tetraazacyclododecane).

A new supramolecular complex (Ru(Zn2L4)3) was designed and synthesized as a luminescence sensor for inositol 1,4,5-triphosphate (IP3), which is one of the important second messengers in intracellular signal transduction, and its achiral model compound, cis,cis-1,3,5-cyclohexanetriol triphosphate (CTP3), by a ruthenium(II)-templated assembly of three molecules of a bis(Zn2+-cyclen) complex having a 2,2-bipyridyl linker (Zn2L4). Single-crystal X-ray diffraction analysis of a racemic mixture of Ru(Zn2L4)3 showed that three of the six Zn2+-cyclen units are orientated to face the opposite side of the molecule with three apical ligands (Zn2+-bound HO-) of each of the three Zn2+ located on the same face. 1H NMR and UV titrations of Ru(Zn2L4)3 with CTP3 indicated that Ru(Zn2L4)3 forms a 1:2 complex with CTP3, (Ru(Zn2L4)3)-((CTP3)6-)2, in aqueous solution at neutral pH. In the absence of guest molecules, Ru(Zn2L4)3 (10 microM) has an emission maximum at 610 nm at pH 7.4 (10 mM HEPES with I = 0.1 (NaNO3)) and 25 degrees C (excitation at 300 nm). An addition of 2 equiv of CTP3 induced a 4.2-fold enhancement in the emission of Ru(Zn2L4)3 at 584 nm. In this article, we describe that Ru(Zn2L4)3 is the first chemical sensor that directly responds to CTP3 and IP3 and discriminates these triphosphates from monophosphates and diphosphates. The photodecomposition of Ru(Zn2L4)3, which is inhibited upon complexation with CTP3, and the stereoselective complexation of chiral IP3 by Ru(Zn2L4)3 are also described.

Cyclohexanes↗