- The ultraviolet spectra of matrix isolated disulfur monoxide and sulfur dioxide
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The absorption spectrum of disulfur monoxide was observed in matrices at 20°K. All 18 observed bands of the (0, 0, ν3) - (0, 0, 0) progression fit the equation G(ν3′) = 29 070 + 426 (ν3′ + 1 2) - 4.80 (ν3′ + 1 2)2 + 0.075 (ν3′ + 1 2)3. The matrix data was used to reassign the reported gas-phase data and to deduce ν2′ and ν2″. The absorption spectrum of sulfur dioxide in a krypton matrix at 20°K is tentatively assigned to a progression A(ν1, ν2, 0) ← X(0, 0, 0). The SO2 a-X phosphorescence, excited by absorption of light in either the C or A system, is strongly enhanced in the matrix. T00, ν1 and ν2 shifts are listed for solid argon, krypton, xenon, nitrogen, methane, SF6, and C4F8. The phosphorescence intensity is strongly temperature dependent. The temperature-intensity curves are consistent with an energy transfer model involving interaction of the SO2 triplet state with the lattice vibration.
- Phillips, L.F,Smith, J.J,Meyer, B
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- 7H-pyrrolo[2,3-d]pyrimidine derivatives
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The invention relates to 7H-pyrrolo[2,3-d]pyrimidine derivatives of formula I wherein the symbols and substituents are as defined in the description, to processes for the preparation thereof, to pharmaceutical compositions comprising such derivatives and to the use of such derivatives—alone or in combination with one or more other pharmaceutically active compounds—for the preparation of pharmaceutical compositions for the treatment especially of a proliferative disease, such as a tumour.
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- Hydroxamic acid derivatives as proteinase inhibitors
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Compounds of formula (I) are matrix metalloprotemase inhibitors wherein X represents a carboxylic acid group —COOH, or a hydroxamic acid group —CONHOH;R2represents a radical of formula (II): R3—(ALK)m—(Q)p—(ALK)n., and W represents a cyclic amino radical of formula (IIIA) or (IIIB):
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- Method for the preparation of 2-chloro sulfinyl azetidinones
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An improved method for the preparation of 2-chloro sulfinyl azetidin-4-one of the formula: STR1 wherein R is: hydrogen; C1 -C3 alkyl; halomethyl; cyanomethyl; phenyl; substituted phenyl; phenoxy, benzyloxy- or substituted benzyl; a group of the formula R2 --O--wherein R2 is t-butyl, 2,2,2-trichloroethyl, benzyl or substituted benzyl; a group of the formula R3 --(O)n --CH2 wherein R3 is phenyl or substituted phenyl. The 2-chlorosulfinylazetidin-4-one is prepared by reacting a penicillin sulfoxide ester of the general formula STR2 wherein R and R1 have the meanings defined above with an N-chloro halogenating agent in an inert organic solvent. The reaction is carried out in the presence of an acid scavenging amount of a phosphate or hydrogen phosphate of an alkali metal, alkaline earth metal, ammonium, quaternary ammonium or mixtures thereof. These compounds find application as intermediates in the production of cefaclor which are powerful anti-bacterial compounds.
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- Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaamino-1-oxo-1λ5,3λ 5-diphosphaz-2-ene, (NH2)2(O)P-N=P(NH2)3
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Coarse crystalline (NH2)2(O)P-N=P(NH2)3 is obtained from a NH3 saturated CH2Cl2 suspension of (NH2)2(O)P-N=P(NH2)3·NH 4Cl at room temperature. (NH2)2(O)P-N=P(NH2)3·NH 4Cl is synthesized by slow addition of Cl2(O)P-N=PCl3 to a solution of NH3 in CH2Cl2 at -78 °C. Excess NH4Cl is removed by treatment with HNEt2 followed by extraction with CH2Cl2. The crystal structure of (NH2)2(O)P-N=P(NH2)3 has been determined by single crystal X-ray methods (P21/c; a = 1462.8(3) b = 944.8(2), c = 1026.9(2) pm, β= 110.69(3)°; Z = 8). In the unit cell there are two crystallographically unique molecules. They form a three dimensional network by intermolecular hydrogen bonding interactions (N-H...N ≥ 313 pm, N-H-...O ≥ 293 pm). The investigation of the thermal properties shows decomposition with evolution of NH3 above 80°C.
- Stock,Schnick
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p. 1079 - 1083
(2007/10/03)
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- Silicate compounds for DNA purification
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The present invention relates to a silicon-containing material which exhibits sufficient hydrophilicity and sufficient electropositivity to bind DNA from a suspension containing DNA and permit elution of the DNA from the material. Generally, the hydrophilic and electropositive characteristics are expressed at the surface of the silicon-containing material. Preferred silicon-containing materials of the present invention include boron silicate, aluminum silicate, phosphosilicate, silica carbonyl, silica sulfonyl and silica phosphonyl. The silicon-containing materials of the present invention are particularly useful in processes for purification of DNA from other cellular components. In these processes, a suspension of cellular components is placed in contact with the silicon-containing material, the silicon-containing material is washed to remove all cellular components other than DNA which are bound to the material, and the bound DNA is eluted from the material. Several of the silicon-containing materials are capable of binding and eluting DNA using only water.
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- Sulfonamides of phenylalkylamines or phenoxyalkylamines processes for their preparation and medicaments containing these compounds
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Compounds of the formula I STR1 in which R1 signifies an aryl, aralkyl or an aralkenyl group, the aryl radical of which can, in each case, be substituted one or more times by halogen, cyano, alkyl, trifluoromethyl, alkoxy, alkylthio, trifluoromethoxy, hydroxyl or carboxyl, m a whole number from 1 to 3, n a whole number from 1 to 5, R2 hydrogen, an alkyl, aralkyl or acyl group, Q a bond or an oxygen atom, R3 hydrogen or a lower alkyl radical which is possibly terminally substituted by carboxyl or by a hydroxyl group and R4 hydrogen, a lower alkyl group with 1-4 C-atoms, which is possibly terminally substituted by carboxyl or hydroxyl, a possibly substituted phenyl, heteroaryl, cycloalkyl or acyl group or a group STR2 in which R5 represents a straight-chained or branched alkyl chain with 1-4 C-atoms which is possibly terminally substituted by carboxyl, alkoxycarbonyl, aminocarbonyl, hydroxyl, mercapto, alkylthio or imidazolyl and Y a carboxyl, an alkoxycarbonyl, aminocarbonyl or cyano, formyl, hydroxymethyl, aminomethyl or ortho ester group, whereby R3 and R4 can also be component of a 5- or 6-membered saturated or unsaturated possibly substituted heterocycle with 1-4 heteroatoms which can be annellated with further ring compounds via one or more bonds, as well as their salts, esters and amides, processes for their preparation and medicaments with thromboxane-antagonistic action which contain these compounds.
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- 5-azolylacetoxymilbemycins as ecto- and endoparasites
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The present invention relates to milbemycin derivatives of the formula I STR1 wherein X is hydrogen or β-halogen, R is methyl, ethyl, isopropyl or sec-butyl and Az is a 5 membered heterocyclic aromatic ring which contains 2-4 nitrogen atoms and is attached in the 1-position and which is unsubstituted or substituted by one or two C1 -C6 alkyl groups. These compounds, and the acid addition salts and metal complexes thereof, are effective pesticides for controlling endo-and ectoparasites, especially for controlling neamatodes which are parasites of animals. The may be obtained by appropriate esterification in 5-position of milbemycin derivatives. The selective β-halogenation of 14,15-epoxymilbemycin derivatives can be effected via the intermediate Δ13,14 -15-hydroxymilbemycins with appropriate halogenating agents.
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- THE LOWER OXIDES OF SULFUR AND RELATED ORGANIC SULFOXIDES
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The preparation, structures, spectra and other properties of organic sulfane oxides, R2SnO (n = 3,4), and dioxides, R2SnO2 (n = 3,4), as well as of the homocyclic sulfur oxides SnO (n=6...10) and SnO2 (n = 7,12) are discussed.All compounds are sulfoxides and contain two or more homonuclear S-S bonds.
- Steudel, Ralf
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- Reversible Isomerization of Cyclo-octasulfur Monoxide; Preparation and X-Ray Crystal Structure of S8O*SbCl5
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The reaction of S8O and SbCl5 in CS2 gave S8O*SbCl5 (71percent yield) which was shown by X-ray crystallography to contain S8O in an isomeric conformation compared with pure S8O which can be recovered from the adduct in its usual conformation by recrystall
- Steudel, Ralf,Sandow, Torsten,Steidel, Juergen
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p. 180 - 181
(2007/10/02)
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- Sulfinyl halides and their preparation from penicillin sulfoxides
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A penicillin sulfoxide ester is reacted with an N-chloro halogenating agent at a temperature of from about 75° C. to about 135° C. to produce a novel 2-chlorosulfinylazetidin-4-one intermediate. The intermediate can be treated with stannic chloride to produce a 3-exomethylenecepham sulfoxide.
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- Method of preparation of 3-methylenecephams
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Penicillin sulfoxide derived azetidinone sulfinyl chlorides and related sulfinic acid derivatives are cyclized to 3-methylenecephams by reaction with Friedel-Crafts catalysts or metathetic cation forming agents.
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- Preparation of desacetoxy-cephalosporin sulfoxides from penicillin sulfoxides
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A penicillin sulfoxide ester is reacted with sulfuryl chloride at a temperature of from about 75°C. to about 120°C. to produce a novel 2-chlorosulfinyl-azetidin-4-one intermediate, which intermediate is treated with an alkaline reagent to produce a desaceetoxycephalosporin sulfoxide.
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