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Crude Reaction Mixture (crude + reaction_mixture)
Selected AbstractsSynthesis and Functionalization of Germanium Triphenylcorrolate: The First Example of a Partially Brominated CorroleEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 16 2007Sara Nardis Abstract Ge complexes of 5,10,15-triphenylcorrole were prepared in refluxing dry DMF using GeCl4 as the source of Ge. Chromatographic separation of the crude reaction mixture afforded the ,-oxo dimer 1 and the methoxy derivative 2a. The corresponding chloride 2b can be obtained by treatment of 1 or 2a with HCl. The reaction of 2a with Br2 in CHCl3/py afforded the hexabromo derivative 3 as the main product, giving the first indication of the regioselective substitution of pyrroles B and C on the corrole ring. The fully brominated open-chain tetrapyrrole 4 was also characterized as a reaction by-product. Different partially brominated Ge complexes 5 and 6 have been obtained by variation of reaction conditions, while the heptabromo derivative was obtained in a mixture with the corresponding fully brominated Gecorrole. Photophysical characterization of Ge corrolates confirmed the high fluorescence quantum yield of such complexes, and also led to the first observation of phosphorescence emissions from corrole complexes. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source] Simplification of separation of the reaction mixture after transesterification of vegetable oilEUROPEAN JOURNAL OF LIPID SCIENCE AND TECHNOLOGY, Issue 4 2008Martin Hájek Abstract A heterogeneous reaction mixture is formed by transesterification of vegetable oils. The reaction mixture contains mainly methyl esters of higher fatty acids and glycerol. From this mixture, biodiesel is gained by spontaneous sedimentation in the gravitational field. The sedimentation can be considerably accelerated by controlled addition of water. It was found that addition of small amounts of water to the crude reaction mixture significantly affected the mixture, and substantial changes in the speed of the separation took place. Considerable differences in the composition and quality of the ester and glycerol phases occurred. The optical properties (transmittance and refractive indices) of the heterogeneous reaction mixture are changed after addition of water; this change can be observed spectrophotometrically. This method is applicable to all types of vegetable oils including waste frying oils. [source] Improved Synthesis and Isolation of 2,- O -Methyladenosine: Effective and Scalable Enzymatic Separation of 2,/3,- O -Methyladenosine RegioisomersEUROPEAN JOURNAL OF ORGANIC CHEMISTRY, Issue 19 2009Saúl Martínez-Montero Abstract An efficient separation of a mixture of 2,/3,- O -methyladenosine regioisomers (1 + 2; 1:1) has been developed by selective enzymatic acylation using immobilized Pseudomonas cepacia lipase (PSL-C) in combination with acetonoxime levulinate as acyl donor. The 3,-hydroxy group of 2,- O -methyladenosine (1) was acylated with high selectivity (ca. 70,%), whereas an equal amount of 3,- O -methyladenosine (2) in the same solution resulted in minor acylation of 5,-hydroxy group (ca. 8,%). The differential behavior of both regioisomers towards enzymatic acylation allowed to develop a separation protocol. Upon extraction of the acylated products, the 3,- O -methyladenosine was isolated in 81,% yield and 97,% purity from the aqueous layer. Hydrolysis of acylated products in organic layer furnished 2,- O -methyladenosine in 67,% yield and 99,% purity. The separation process was successfully applied to the crude reaction mixture of methylated products (ca. 3:1 of 1/2) on 5-g scale. We also report on the use of methyl p -toluenesulfonate as a safe reagent for 2,- O -methylation of adenosine.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Cell-free synthesis of 15N-labeled proteins for NMR studiesIUBMB LIFE, Issue 9 2005Kiyoshi Ozawa Abstract Modern cell-free in vitro protein synthesis systems present powerful tools for the synthesis of isotope-labeled proteins in high yields. The production of selectively 15 N-labeled proteins from 15 N-labeled amino acids is particularly economic and yields are often sufficient to analyze the proteins very quickly by two-dimensional NMR spectra recorded of the crude reaction mixture without concentration or chromatographic purification of the protein. We review methodological aspects of cell-free in vitro protein synthesis based on an Escherichia coli cell extract, in particular with regard to the production of 15 N-labeled proteins for analysis by NMR spectroscopy. IUBMB Life, 57: 615-622, 2005 [source] Quaternary Ammonium-Supported Scavenger Reagents for Acids and ElectrophilesEUROPEAN JOURNAL OF ORGANIC CHEMISTRY, Issue 1 2004Noha Ghanem Abstract The present article describes how we devised new quaternary ammonium-supported quench reagents (TAMA-Cl and BAX-sulfate) for scavenging acids and excess electrophiles from crude reaction mixtures. TAMA-Cl is liquid at room temperature, but is very glutinous and has to be used in aqueous solution. It removes unchanged electrophiles very efficiently. An aqueous preparation of TAMA-Cl may be easily added in automated syntheses, and high-throughput phase-separation techniques should allow purification of scavenger-containing reaction mixtures. However, workup with TAMA-Cl is more complex than simple filtration. Recognizing this major advantage of solid-phase syntheses, we designed BAX-sulfate, a highly crystalline scavenger reagent that allows reaction workup to be simplified to a single filtration and evaporation of solvent. BAX-sulfate reacts with electrophiles, quenches acids and precipitates quantitatively when diethyl ether is added. It even precipitates from methanol solutions. With BAX-sulfate the workup stage uses simple filtration to make crude separations. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004) [source] | |||||||||||||