Coordination compounds of Co(II), Ni(II), and Cu(II) valerates and benzoates with semicarbazide

Complexes of Co(II), Ni(II), and Cu(II) valerates and benzoates with semicarbazide were prepared. The compounds were characterized by chemical analysis, X-ray phase analysis, IR spectroscopy, diffuse reflection spectroscopy, and thermal gravimetric analysis.     

Interaction between indigo and adsorbed protein as a major factor causing backstaining during cellulase treatment of cotton fabrics

A model microassay system was developed to measure indigo backstaining on cotton fabrics in the presence of enzymes on a small laboratory scale. Backstaining indexes for 11 cellulase samples were measured, and the enzymes were ranked from lower to higher backstaining. Two multienzyme cellulase preparations were separated into fractions using chromatofocusing on a Mono P column. Adsorption ability and backstaining properties of purified enzyme fractions were studied. Evidence was obtained that protein adsorption on cotton fabrics is a crucial parameter causing backstaining (both for crude cellulase samples and purified enzyme components).     

Evaluation of cellulase preparations for hydrolysis of hardwood substrates

Seven cellulase preparations from Penicillium and Trichoderma spp. were evaluated for their ability to hydrolyze the cellulose fraction of hardwoods (yellow poplar and red maple) pretreated by organosolv extraction, as well as model cellulosic substrates such as filter paper. There was no significant correlation among hydrolytic performance on pretreated hardwood, based on glucose release, and filter paper activity. However, performance on pretreated hardwood showed significant correlations to the levels of endogenous β-glucosidase and xylanase activities in the cellulase preparation. Accordingly, differences in performance were reduced or eliminated following supplementation with a crude β-glucosidase preparation containing both activities. These results complement a previous investigation using softwoods pretreated by either organosolv extraction or steam explosion. Cellulase preparations that performed best on hardwood also showed superior performance on the softwood substrates.     

Polymeric Structure and Solid ~(31)P, ~(113)Cd NMR Spectra of Cadmium(II) Dialkyldithiophosphate (Alkyl = n-butyl and i-butyl)

Owing to the particular affinity toward metal ion and changeable dentation, dialkyldithiophosphates are commonly used ligands in preparation of the transition metal complexes with variable structures1. For instances relevant to this work, the IIB metal complexes defined crystallographically so far have provided the examples as follows2-12 (Scheme 1). Scheme 1 The frameworks of IIB metal complexes of dialkyldithiophosphate MMMMMMMMMM a b c d …     

Detection of explosives on solid surfaces by thermal desorption and ambient ion/molecule reactions

A simple, fast and direct method is presented for detecting traces of solid explosives on cotton swabs or in particulate samples: ions are transferred into a mass spectrometer after thermal desorption and corona discharge chemical ionization in ambient air; specificity is enhanced using ambient ion/molecule reactions or by conventional tandem mass spectrometry.     

Synthesis in the phenothiazine series

Quaternary salts of imidazo[4,5,1-k,l]phenothiazine were reduced with potassium borohydride to 1,2-dihydro-2-methylimidazo[4,5,1-k,l]phenothiazine, which was converted to 1,2 dihydro-2-methylimidazo[4,5,1-k,l]phenothiazine-1-thione and 1-methylamino-10-formylphenothiazine. The latter was hydrolyzed to 1-methylaminophenothiazine, which was also obtained by reduction of methyl phenothiazine-1-carbamate. The PMR and IR spectra of some of the derivatives are discussed.See [1] for communication XXXV.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 372–374, March, 1974.     

Application of water-soluble polymers as modifiers in electrophoretic analysis of phenols

A review of application of water-soluble cationic, anionic and nonionic polymers as pseudostationary phases in capillary electrophoresis (CE) and micellar electrokinetic capillary chromatography (MEKC) is presented. The effect of the structure of the polymers on the selectivity and efficiency of separation is discussed. A novel specially designed cationic polymer, 2,10-ionene, has been used for the separation of phenols. The polymer has hydrophilic and hydrophobic parts in its backbone. The polymer shows the best selectivity as a modifier in capillary zone electrophoresis (CZE)-mode, which allows the selective determination of both hydrophilic and hydrophobic phenols.     

Low-temperaturic template synthesis of macrocyclic cobalt(III) chelates with (N,N,S,S)-donor atomic ligands in the cobalt(II)–dithiooxamide-formaldehyde and cobalt(II)–dithiooxamide-glyoxal systems in the Co2[Fe(CN)6]-gelatin-immobilized matrices

The complexing processes in the triple cobalt(II)–dithiooxamide-formaldehyde and cobalt(II)–dithiooxamide-glyoxal systems taking place in the cobalt(II)hexacyanoferrate(II) gelatin-immobilized matrix in contact with aqueous alkaline solutions (pH ca. 12) containing (dithiooxamide+formaldehyde) and (dithiooxamide+glyoxal), have been studied. Template synthesis leading to macrocyclic coordination compounds with tetradentate N,N,S,S-donor ligands-(2,8-dithio-3,7-diaza-5-oxanonan-dithioamide-1,9) and (2,7-dithio-3,6-diazaoctadien-3,5-dithioamide-1,8) with Co^II–Co^III redox-process occurs under these specific conditions where dithiooxamide, formaldehyde and glyoxal are the ligand synthons.     

Asymmetrical nonbridgehead nitrogen-17: Complete separation into antipodes and absolute configuration of chiralic n-alkoxyisoxazolidines

trans-Stereospecificity of the amidation of 1-alkoxyisoxazolidine-3,3-dicarboxylic ester (1) has been elucidated. Alkaline hydrolysis of monester 4 yielded the salt 6 which after its ion exchange in the form of S(?) and R-(+)-phenylethylammonium salts was completely separated into the enantiomeric salts (+10 and ?10). Esterification and amidation of these salts afforded antipodes 2 S-( +12) and 2 R-( ?12) containing only a nitrogen asymmetric center. Optical purities of the products were established on the basis of their NMR spectra with shift-reagent. Molecular and crystal structure as well as an absolute configuration of +10 were detected by means of X-ray analysis.     

Reactions of 4,7‐dihydro‐1,2,4‐triazolo[1,5‐a]pyrimidines with α,β‐unsaturated carbonyl compounds

The reaction of 5,7‐diphenyl‐4,7‐dihydro‐1,2,4‐triazolo[1,5‐a]pyrimidine ( 1 ) with α,β‐unsaturated carbonyl compounds 2a‐f led to the formation of the alkylated heterocycles 3a‐f (Figure 1). However, the reaction of 5‐methyl‐7‐phenyl‐4,7‐dihydro‐1,2,4‐triazolo[1,5‐a]pyrimidine ( 5 ) with 2a‐c yielded under the same conditions the triazolo[5,1‐b]quinazolines 6a‐c (Figure 3). In this case, the alkylation is followed by a cyclocondensation. The structure elucidation of the products is based on ir, ms, ¹H and ¹³C nmr measurements and on an X‐ray diffraction study.