Synthesis of a flav-3-en-3-ol via cinnamylphenol

Vinyl quinone methide ($\text{1}$) reacts with polyphenols to give cinnamylphenols ($\text{4}$) and neo-flavanoids ($\text{5}$). Oxidation of cinnamylphenol ($\text{4}$b) leads to malvidin ($\text{10}$) via the isolated intermediate flav-3-en-3o1 ($\text{8}$b).     

Laser-induced fluorescence of high-temperature vapor complexes of ErCl3 with AlCl3, GaCl3 and InCl3

Laser excitation of equilibrium vapor mixtures ErCl₃(s)-ACl₃(g) (A = Al, Ga, In) at 475–1100 K gives rise both to resonance fluorescence from the f → f Er³⁺ transitions of the Er-Cl-A vapor complexes, and to Raman scattering due to the vibrational modes of the ACl₃ vapor. The laser-induced fluorescence from the ⁴F_{$\text{9}\text{2}$}, ⁴S_{$\text{3}\text{2}$} and ²H_{$\text{11}\text{2}$} states has been investigated at different temperatures and excitation.     

Heat capacity and thermodynamic properties of ramsdellite,Li2Ti3O7, and spinel,Li43Ti53O4

The heat capacity and heat content Li_{$\text{4}\text{3}$}Ti_{$\text{5}\text{3}$}O₄ and Li₂Ti₃O₇ have been measured in the temperature range 198—960 K. The lattice and dilation contributions to the heat capacity have been estimated. The standard thermodynamic functions and the high temperature enthalpy and entropy have been derived. The lattice heat capacity of Li_{$\text{4}\text{3}$}Ti_{$\text{5}\text{3}$}O₄ spinel appears to be consistent with the phonon model put forward by Grimes.     

BH3 THF reduction of 3-methylisoxazolo [4,5-c]pyridines

3-Methylisoxazolo[4,5-c]pyridine $\text{1}$ on reduction with BH₃:THF gave, via the isolable complex $\text{4}$, the tetrahydroisoxazolopyridine $\text{5}$. The presence of two chlorine atoms at the 4 and 6 positions directed borane attact to the isoxazole ring, yielding the aminoethylpyridine $\text{8}$. Both types of reduction were obtained with 6-chloroisoxazolo[4,5-c]pyridine $\text{7}$.     

Thermolysis of n-(o-azidobenzoyl)-iminopyridinium ylide: a new route to 3h-indazol-3-one

3$\text{H}$-Indazol-3-one has been generated by thermolysis of $\text{N}$($\text{o}$-azidobenzoyl)iminopyridinium ylide and trapped as its Diels-Alder cycloadducts with several dienes.     

Base-induced intramolecular cyclisation of N-(o-azidobenzoyl)-arylamines. A new synthesis of 2-aryl-1,2-dihydro-3H-indazolin-3-ones

In strong base, e.g., sodium hydride in dimethylformamide, $\text{N}$-($\text{o}$-azidobenzoyl)arylamines cyclise in high yield to 2-aryl-1,2-dihydro-3$\text{H}$-indazolin-3-ones.     

A stereoselective 3-endo-alkyl-5,6-dehydroisoquinuclidine synthesis.

Cycloaddition of N-carbethoxy-2-alkyl-1,2-dihydropyridines $\text{4}$ with phenylvinylsulfone $\text{5}$ provides adducts $\text{6}$, which upon desulfonylation afford stereoselectively N-carbethoxy-3-$\text{endo}$- alkyl-5,6-dehydroisoquinuclidines $\text{1}$.     

Observation of nonlinearity and asymmetry in energies of EPR transitions of 160Gd3+ in La(C2H5SO4)3 · 9D2O at low magnetic fields

The energies of EPR transitions of ¹⁶⁰Gd³⁺ in La(C₂H₅SO₄₃ · 9D₂O at 77.2 K are observed to be nonlinear functions of field at low fields. The + $\text{3}\text{2}$, + $\text{1}\text{2}$ and ?$\text{3}\text{2}$, ?$\text{1}\text{2}$ transition energies converge asymmetrically below 10 G and differ by only ≈ MHz at the lowest fields employed.     

Synthesis of 2β-fluoro-1α-hydroxyvitamin D3

2β-Fluoro-1α-hydroxyvitamin D₃($\text{3}$) was prepared from 1,2α-epoxy-cholest-5-en-3β-yl tetrahydropyranyl ether($\text{1a}$ via 2β-fluorocholest-5-ene-1α, 3β-diol($\text{2}$).     

Dedoublement et configuration absolue de la methyl-3 δ3(3a)-hydrindenone-4.etude de l'isomerisation en methyl-3 δsu3a(7a)-hydrindenone-4.

During the hydrogenation of the Δ^3(3a)-4-hydrindenones $\text{1}$ or $\text{3}$ on Pd or Ni, we observe a shift of the double bond to Δ^3a(7a)-4-hydrindenones $\text{2}$ and $\text{4}$. The absolute configuration established for ketones $\text{1}$ and $\text{2}$ shows that the reaction is a suprafacial process. By deuteriation experiments, we observe that the reaction is irreversible and occurs with a molecular hydrogen exchange.     

Synthesis of N-benzoyl L- and D-2,3,6-trideoxy-3-aminoxylo-hexose from non-carbohydrate precursors

The enantiomeric alcohols ($\text{2}$) and ($\text{11}$), obtained from (2$\text{R}$,3$\text{R}$) tartaric acid and, respectively, $\text{L}$-threonine, have been used to construct the C₆, enantiomeric deoxy amino sugar derivatives ($\text{7}$) and ($\text{12}$)     

A convenient synthesis of erythro- and threo-3-fluorophenyl- alanine from a protected glycine synthon

A facile synthesis of the title compounds ($\text{8}$ and $\text{9}$) is described; key steps include the mono-C-alkylation of the glycine Schiff base benzyl ester $\text{1a}$ with α-bromo-α-fluorotoluene, which provides the readily separable fluorinated diastereomers $\text{2a}$ and $\text{3a}$, and the dealkylative hydrolysis of the benzyl esters $\text{2a}$-$\text{5a}$ without concomitant loss of the benzylic fluorine.     

Penicillin-cephalosporin conversion III. A Novel route to 3-chloromethyl-Δ3-cephems

Synthesis of 3-chloromethyl-Δ³-cephems $\text{3}$ from 4-arenesulfonylthioazetidin-2-ones $\text{1}$, derived from penicillins G and V, has been achieved by the electrolytic ene-type chlorination of $\text{1}$ in a CHC1₃-aqueous NaCl-H₂SO₄-(Pt electrodes) system and subsequent ring closure with NH₃ in DMF.     

A stereocontrolled synthesis of Z and E terminal dienes from pinacol E-1-trimethylsilyl-1-propene-3-boronate

Pinacol $\text{E}$-1-trimethylsilyl-1-propene-3-boronate reacts with aldehydes to form (±)-($\text{R}$*,$\text{S}$*)-3-trimethylsilyl-4-hydroxy-1-alkenes, which can be deoxysilylated stereoselectively to either 98% $\text{Z}$ or 99% $\text{E}$ 1,3-dienes, including the separate components of the red bollworm moth pheromone.     

The synthesis of 3-vinylindoles and 11H-5-cyanobenzol[a]carbazole

The synthesis of 3-vinylindoles through Wadsworth Emmons reactions with 3-formyl and 3-acylindoles is described. Although 3-formylindoles react directly with phosphonate derivatives, 3-acylindoles need prior activation by N-sulphonation. 11$\text{H}$-5-Cyanobenzo[$\text{a}$]carbazole has been prepared by the oxidative cycloaddition of $\text{E}$-3-(indol-3′-yl) propenotrile and benzyne.     

IPSO-substitutions. Reactions of 3-substituted indoles with benzoylperoxide

3-substituted indoles with benzoylperoxide led to the 3-benzoyloxy derivative. The react$\text{i}$on is discussed in terms of homolytic $\text{ipso}$-substitution.     

X-ray structure determinations of the solid state conformations of tri-o-carvacrotide and of tri-3- and tri-6-methylthiosalicylides

In the solid state, tri-6-methylthiosalicylide ($\text{5}$) adopts only $\text{one}$ helical conformation, tri-3-methylthiosalicylide ($\text{4}$) exists as $\text{both}$ enantiomeric helical conformations, and tri-$\text{o}$-carvacrotide ($\text{2}$) provides the first example of the unique situation where $\text{both}$ enantiomeric propeller conformations and $\text{both}$ enantiomeric helical conformations coexist.     

Structure cristalline du phosphatoantimonate K3Sb3P2O14

K₃Sb₃P₂O₁₄ crystallizes in the rhombohedral system, space group $\text{R}\text{3}\text{m}$ with a = 7.147(1) Å, c = 30.936(6) Å, Z = 3. The structure was determined from 701 reflections collected on a Nonius CAD4 automatic diffractometer with $\text{Mo}\text{K}\text{α}$ radiation. The final R index and the weighted R_w index are 0.033 and 0.042, respectively. The structure is built up from layers of SbO₆ octahedra and PO₄ tetrahedra sharing corners. The potassium ions are situated between the (Sb₃P₂O₁₄)^3? covalent layers.     

Vibrational study of the unusual phase sequence in Tl3Cr(SO4)3: A compound containing [Cr(SO43−3]∞ columns

The polarized Raman spectra of small single crystals of Tl₃Cr(SO₄)₃ have been recorded using the Raman microprobe technique in the temperature range 295–660 K. The behavior of the external modes is analyzed on polycrystalline samples with conventional Raman spectrometer from 100 K to the decompositon temperature 660 K. Analysis of the spectra, in connection with dielectric measurements and X-ray data show that Tl₃Cr(SO₄)₃ undergoes the following space group phase sequence

$\text{P2}{}_1\text{c}\text{→}\text{340}\text{K}\text{R}\text{3}\text{→}\text{450}\text{K}\text{R3c}\text{→}\text{630}\text{K}\text{R}\text{3}\text{c}$

in accordance with the point group relationship

$\text{2}\text{m}\text{→}\text{3}\text{→3m→}\text{3}\text{m}$

     

Cis-trihetero-tris-σ-homobenzenes as tridentate ligands - X-ray crystal. Structure analyses of the Co(C6H9N3)2(NO3)3 and Ba(C6H6O3)4(ClO4)2-complexes

According to X-ray crystal structure analyses “cis-benzenetrisimine” ($\text{2}$) and “cis-benzenetrioxide” ($\text{1}$) act as tridentate ligands in their 2:1- and 4:1-complexes $\text{7}$ (Co(C₆H₉N₃)₂(NO₃)₃) and $\text{8}$ (Ba(C₆H₆O₃)₄(ClO₄)₂), resp. The latter is the rare example of an organic complex with the (approximate) T-symmetry.