Silicon-29 diffusion-ordered NMR spectroscopy (DOSY) as a tool for studying aqueous silicates

The first use of silicon-29 diffusion-ordered NMR spectroscopy (DOSY) is reported, in a study of the speciation of aqueous silicates.     

A Simulation Approach to Cost Estimation in the Project Contracting Industry

In the project contracting industry (particularly in Third World and developing economies) one of the basic requirements for a company to produce a bid is an accurate estimate of the overall costs. A typical contract will involve several hundred quotes from different suppliers, and some of the figures will be inherently more risky than others.This paper looks at the effect of component price uncertainties on the overall cost of a project and develops a company-based simulation model to evaluate this. The basic data is derived from the individual expertise existing within the company, and this is statistically tested for consistency.The application of the simulation model is demonstrated, and it is also used to test some simple hypotheses about the existing modus operandi.     

Synthesis,alkylation, and molecular and crystal structure ofN-methylmorpholinium 6-amino-3,5-dicyano-1,4-dihydropyridine-4-spirocyclohexane-2-thiolate

The reaction of cyano(cyclohexylidene)thioacetamide with cyanothioacetamide or malononitrile andN-methylmorpholine yieldsN-methylmorpholinium 6-amino-3,5-dicyano-1,4-dihydropyridine-4-spirocyclohexane-2-thiolate. Its structure was established based on the results of alkylation and X-ray structural analysis.Deceased.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 2535–2540, October, 1996.     

Validated ion-exclusion chromatographic method for citrate and acetate in medical fluids

In this paper we describe the development and validation of a solid-phase extraction procedure, followed by ion-exclusion chromatographic determination of citrate and acetate in medical fluids. The medical fluids contained trace levels of non-polar compounds, which were not of interest for the purposes of assay requirements, but due to their strong affinity towards the ion-exclusion chromatography column necessitated a 180-min long runtime to elute. The developed SPE procedure, based on trapping the hydrophobic compounds, on a reversed-phase material, while allowing analytes of interest elute off unretained, shortened the runtime to 35 min. The procedure is simple since it has only two steps, conditioning of the SPE cartridge with acetonitrile and treating the sample. The SPE procedure followed by ion-exclusion chromatographic determination was successfully validated per the International Conference on Harmonization (ICH) guidelines in terms of specificity, accuracy as recovery versus untreated sample, precision, range, linearity of response, ruggedness, stability of treated samples, and robustness. The validation data showed that the method is specific, accurate, precise, rugged, and robust. The validated method has been routinely used in the manufacturing environment.     

Pyrazolines — Derivatives of 2-nitrochalcone

By the reaction of 2-nitrochalcone with hydrazine hydrate, 5-(2-nitrophenyl)-3-phenyl-1H-2-pyrazoline (I) and the hydrazone of 3-(5-(2-nitrophenyl)-3-phenyl-2-pyrazolin-1-yl)-3-(2-nitrophenyl)propiophenol (II) have been prepared. The acylation of both compounds I and II leads to N-acyl derivatives of the first. The acylating ability of formamide and N,N-dimethylformamide was observed in reactions with pyrazoline I. An x-ray structural study was carried out on compound II.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 360–366, March, 1993.     

Ecdysteroids of a culture of tissues and cells ofAjuga turkestanica

The possibility has been studied of obtaining ecdysteroids — ecdysterone and turkesterone — with the aid of a culture of the tissues and cells of the plantAjuga turkestanica. Conditions have been selected under which the yield of ecdysteroids in the culture of tissues and cells is comparable with amounts of the same substances in the organs of the whole plant.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 51–52, January–February, 1990.     

Acetals of lactams and acid amides. 53. Eamidines in the synthesis of pyridine and pyrimidine

The reaction of -cyano--aminocrotonic ester with DMFA diethylacetal gives 1-ethoxycarbonyl-1-cyano-2-(N-dimethylaminomethylene)-amino-4-dimethylaminobutadiene, the reaction of which with ammonium acetate and amines leads to 4-methylenepyrimidine derivatives. Condensation of -cyano--aminocrotonic ester with dimethylacetamide dieethylacetal gave 2-(ethoxycarbonylcyano)methylene-4-dimethylamino-6-methylpyridine. It was found that in an alkaline medium, 1-benzyl-4-(ethoxycarbonylcyano) methylenepyrimidine recyclizes into 1-benzyl-3-cyano-4-amino-2-pyridone.For Communication 52, see [1].Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 8, pp. 1109–1114, August, 1988.