Excess reagent method

Caution Carry out all procedures in a well-ventilated hood, wear disposable vinyl or latex gloves, and chemical-resistant safety goggles. 

Apparatus for azeotropic distillation singlenecked round-bottomed flasks, condenser, distillation head, thermometer, and adapter 

Preparation-. 1,2-Diaminoethane and methyl acrylate are freshly distilled prior to use. 

The following reaction mixtures must be cooled to 0°C before adding together. All reaction mixtures must be kept under a blanket of nitrogen at all times. 

Synthesis of star-branched ester-terminated precursor  

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DIVERGENT SYNTHESIS OF PAMAM DENDRIMERS VIA EXCESS REAGENT METHOD PREPARATION OF ESTER TERMINATED PAMAM STAR-BRANCHED PRECURSOR [NH2-(CH2)2 6-NH21 (G = -0.5) STAR-PAMAMICO E) [1]... 

Limited-reagent methods measure unoccupied antibodies therefore, optimal sensitivity is achieved as antibody approaches zero. Excess-reagent methods measure occupied antibodies therefore, optimal sensitivity is achieved as antibody approaches infinity. Table 1 compares the general features of these two... 

The advantages of this method are a short reaction time and the nonfluorescence of the OPA reagent. Therefore, excess reagent must not be removed before the chromatography stage. Using this method, it is possible to measure tryptophan, but not secondary amino acids such as proline or hydroxyproline. Cysteine and cystine can be measured, but because of the low fluorescence of their derivatives, they must be detected using an UV system, or alternatively oxidized to cysteic acid before reaction. 

Kwakman et al. [65] described the synthesis of a new dansyl derivative for carboxylic acids. The label, N- (bromoacetyl)-A -[5-(dimethylamino)naphthalene-l-sulfonyl]-piperazine, reacted with both aliphatic and aromatic carboxylic acids in less than 30 min. Excess reagent was converted to a relatively polar compound and subsequently separated from the derivatives on a silica cartridge. A separation of carboxylic acid enantiomers was performed after labeling with either of three chiral labels and the applicability of the method was demonstrated by determinations of racemic ibuprofen in rat plasma and human urine [66], Other examples of labels used to derivatize carboxylic acids are 3-aminoperylene [67], various coumarin compounds [68], 9-anthracenemethanol [69], 6,7-dimethoxy-l-methyl-2(lH)-quinoxalinone-3-propionylcarboxylic acid hydrazide (quinoxalinone) [70], and a quinolizinocoumarin derivative termed Lumarin 4 [71],... 

Conditions Method A Epoxidation using Sharpless reagent method B addition of 0.05-0.1 equivalent of calcium hydride and 0.1-0.15 equivalent of silica gel to the Sharpless reagent, ee = Enantiomeric excess. 

The procedures described are based on improved modifications from original publications [4-8]. They focus on the divergent excess reagent syntheses of dendri-poly(amidoamines) using various alkylenediamine cores. Examples of both divergent in situ branch cell methods, as well as divergent preformed branch cell methods are presented. 

The colorimetric methods depend on a chemical reaction or interaction between the protein and the colorimetric reagent. The resulting generation of a chro-mophore, whose intensity is protein-concentration dependent, can be quantified using a spectrophotometer. Beer s Law is employed to derive the protein concentration from a standard curve of absorbances. Direct interaction of the protein with a chromogenic molecule (dye) or protein-mediated oxidation of the reporter molecule generates a new chromophore that can be readily measured in the presence of excess reagent dye. 

Solution-phase synthesis [5] often needs purification or clean-up procedures after each reaction step to remove excess reagent. These methods include scavenging, extractions and associated plate transfers. All these procedures cause the loss of the desired compound. Although the purity can be improved after treatment, the chemical yield is seriously compromised. In contrast, SPOS has a unique advantage in purifying bound compound without losing compound mass. However, if the reaction is not complete at each step, the side products will form on resin and they cannot be removed while bound to the resin. The final yield and purity wiU both suffer as a result. A 90% yield for a four-step synthesis wiU produce the final product in a disappointing 65% yield. 

Methods and Since elemental tellurium is separated during the reaction, the debromination can be performed using only catalytic amounts of tellurium, the reagent being continuously regenerated at the expense of excess Rongalite (method E) and (Et0)2P(0)Na (method E). 

In general, solid-phase synthesis, rather than solution-phase synthesis, can be the preferred method for the generation of combinatorial libraries because of the greater abihty to automate a solid-phase protocol, primarily due to the use of excess reagents in solution to effect cleaner reactions and to the ease of workup by simple filtration. The solid-phase method of peptide synthesis has had many notable successes. However, the preparation of peptides containing more than 20 amino acids in length using the solid-phase technique often causes major problems in that very extensive purification of the final product is needed. 

Table 14 presents the chemical shifts of l9F-signal pairs of selected diastereomeric imidazolidines. The advantages of the above method can be summarized as follows high chemose-lectivity-ketones do not react C2 symmetry means a diastereomeric control excess reagent can be easily removed generally, an excellent separation of H-, l3C- and, 5F-NMR signals of the diastereomers is observed. 

The oxidation of carboxylic acids with H202 and an acid catalyst is the best general method for the preparation of peroxy acids.450 The most common catalyst for aliphatic R is concentrated sulfuric acid. The reaction is an equilibrium and is driven to the right by removal of water or by the use of excess reagents. For aromatic R the best catalyst is methanesulfonic acid, which is also used as the solvent. 

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