Methods of isolating

Secondary and tertiary amines are not generally prepared in the laboratory. On the technical scale methylaniline is prepared by heating a mixture of aniline hydrochloride (55 parts) and methyl alcohol (16 parts) at 120° in an autoclave. For dimethylaniline, aniline and methyl alcohol are mixed in the proportion of 80 78, 8 parts of concentrated sulphuric acid are added and the mixture heated in an autoclave at 230-235° and a pressure of 25-30 atmospheres. Ethyl- and diethyl-anihne are prepared similarly. One method of isolating pure methyl- or ethyl-aniline from the commercial product consists in converting it into the Y-nitroso derivative with nitrous acid, followed by reduction of the nitroso compound with tin and hydrochloric acid ... 

Ultrapure iodine can be obtained from the reaction of potassium iodide with copper sulfate. Several other methods of isolating the element are known. 

Terbium has been isolated only in recent years with the development of ion-exchange techniques for separating the rare-earth elements. As with other rare earths, it can be produced by reducing the anhydrous chloride or fluoride with calcium metal in a tantalum crucible. Calcium and tantalum impurities can be removed by vacuum remelting. Other methods of isolation are possible. 

Production. Rosin is isolated from pine trees, principally from longleaf Pinuspalustris slash Pinus ellioti and lobloUy pine Pinus taeda. The products are known as gum, wood, or tall oil rosin, based on the method of isolation and the source. 

The last arrangement of voltage feedbaek is the isolated feedback. This is used when the input voltage is eonsidered lethal to the operator of the equipment (>42.5 VDC). The two aeeepted methods of eleetrieal isolation are optical (optoisolator) or magnetic (transformer). This seetion will talk about the more eommon method of isolation, when an optoisolator is used to isolate the lethal portions of the eireuit from the operator portion. The optoisolator s Ct (eurrent transfer ratio (or drifts with temperature, ean degrade slightly with age,... 

Thebaine, CjgHgiOgN. This base, which occurs in opium to the extent of 0-1 to 1 per cent., was first obtained by Pelletier and Thiboumery, who regarded it as isomeric with morphine, and named it paramorphine. It was examined by Kane, who first called it thebaine, and by Anderson, who described a method of isolation and provided the formula given above. It remains in the mother liquor after the removal of morphine and eodeine hydrochlorides in Gregory s process, and in Hesse s method of isolating it from this source is obtained as the acid tartrate. This is crystallised from hot water, and the alkaloid regenerated from it is reerystallised from dilute alcohol, from which it separates in leaflets, or from dry alcohol in prisms, m.p. 193°, — 218-6° (EtOH) or — 229-5°... 

A notable change in methods of isolating alkaloids from plant materials has been described by Applezweig, depending on the use of a suitable ion-exchange material and capable of application on a semi-micro scale or for industrial use. It has been applied to the preparation of the total alkaloids of cinchona bark (totaquina) and according to Sussman, Mindler and Wood, is also used industrially for the recovery of hyoscine. 

Hydroxy-B-homo-5a-cholestan-7-one acetate (54b) A solution of 3/3-hydroxy-5a-cholestan-7-one acetate (51b 5 g mp 146-148°) in dioxane-ethanol (100 ml, 1 1) is placed in a 250 ml three-necked flask equipped with a mechanical stirrer and thermometer and is cooled to 0° (iee-salt bath). Powdered potassium cyanide (7.3 g) is added portionwise with stirring. Acetic acid (8 ml) is then added dropwise with constant stirring over 30 min. The resultant mixture is stirred for 1 hr at 0° C and for an additional 2 hr at room temperature. It is then poured into ice water (200 g ice, 100 ml water) and after standing for 1 hr the precipitate is collected by filtration. The product is dissolved in ether (100 ml), the ether solution is washed with 5% sodium bicarbonate, water and dried over anhydrous sodium sulfate. The filtrate is evaporated at reduced pressure and the solid residue (5.1 g) is crystallized from ethyl acetate (30 ml) to yield 2.8 g of cyanohydrin (52b) mp 160-164° repeated crystallization from the same solvent gives a product mp 164-167°. An alternative method of isolation of the cyanohydrin is used when 100 g or larger quantities are worked up. The reaction mixture is poured directly into a mixture of ice water and sodium bicarbonate, the precipitate (mp 155-156°) is washed well with water, dried and used directly for the next step. 

There are four main methods of isolating boron from its compounds ... 

Good yields of 10-aryl-3,6-dinitroacridones were obtained merely by heating 2,2, 4,4 -tetranitrobenzophenone (419) with an excess of the corresponding aryl amines at 125°C. For example, aniline provided 420 in 80% yield (Eq. 38). The reaction is fairly general for meta- and para-substituted anilines, though it proceeds less readily with orf/io-substituted compounds (79JCS(P1)1364). A method of isolation of the intermediate diarylamine in the synthesis of certain 10-aryl-3,6-dinitroacridones from 2,2, 4,4 -tetranitrobenzophenone has also been described (93JCR(M)2779). 

These are fitted between the cable boxes and the transformer windings and are accessible through a secured cover. Disconnecting chambers can be employed as a method of isolation, but their most common usage is to facilitate phase-to-phase testing of the connected cables. 

The kinetics of a complex catalytic reaction can be derived from the results obtained by a separate study of single reactions. This is important in modeling the course of a catalytic process starting from laboratory data and in obtaining parameters for catalytic reactor design. The method of isolation of reactions renders it possible to discover also some other reaction paths which were not originally considered in the reaction network. 

With two of the concentrations in large excess, the fourth-order kinetic expression has been reduced to a first-order one, with considerable mathematical simplification. The experimental design in which all the concentrations save one are set much higher, so that they can be treated as approximate constants, is termed the method of flooding (or the method of isolation, since the dependence on one reagent is thereby isolated). We shall consider the method of flooding further in Section 2.7. Here our concern is with the data analysis it should be evident that the same treatment suffices for first-order and pseudo-first-order kinetics. 

The most common method of isolation and sample cleanup involves contacting a filtered aqueous solution with an appropriate immiscible organic solvent in a. aboratory separatory funnel of appropriate size. Some specific examples are discussed later. With multicomponent samples a single solvent or solvent mixture is unlikely to extract all components equally causing discrimination. Ihis discrimination may be useful if the solvent discriminates against the extraction of solutes that are not of interest in the analysis. 

Method of Isolation Species and Tissue Chemical Class Reference... 

Allelochemic effects of aquatic macrophytes on algae are discussed. Bloassays of chromatographic fractions from Eleocharls mlcrocarpa Torr. Indicate that oxygenated fatty acids are the causative agents. Methods of Isolation of these materials from aquatic macrophytes and from natural waters are described. Purification and structure determinations show that prominent components of the fraction are C q tri-hydroxycydopentyl and hydroxycydopentenone... 

The oligomer distribution is highly dependent on the method of isolation of the oligomers (TLC, Soxhlet or dissolution/precipitation). Jung and Lee [513] have determined a dimer of 2-phenylbenzoxazole in a polyester resin by means of TLC. A comparative study of the separation of styrene oligomers (up to dodecamers) by TLC and OPLC has appeared [514]. 

Most of the common methods of isolation of heparin (described in sufficient detail in monographs128-30) are based on a procedure, developed by Charles and Scott,31 involving autolysis of the tissue (originally beef liver and beef lung), extraction with alkali, coagulation of proteins by heating, and precipitation of a heparin - protein complex by acidification. Heparin is recovered from the complex by reprecipitation with ethanol, or acetone, or both. Fats are removed by extraction with ethanol, and proteins by treatment with trypsin. Modifications of this proce-... 

However, in a re-investigation of the reaction of benzyne with benzene 39>, it was shown that the original method of isolating benzene-diazonium-2-carboxylate resulted in the contamination of the zwitter-ion with silver salts 40>41). In the absence of silver ions biphenylene, and... 

Use of Excess Concentrations—The Isolation Method. The method of isolation for elucidating the form of the reaction rate expression is based on the simplifications that occur when the concentration of one or more of the reactants appearing in the rate expression is much greater than that called for by the stoichiometry of the reaction. 

A violent explosion occurred after distillation at 47-49°C/60-65 mbar [l],and also during distillation at 48-53°C/66 mbar use of solutions of undistilled material was recommended [2], The compound exploded on one occasion in the solid state after condensation at — 196°C, probably owing to fortuitous tribomechanical shock [3], A similar explosion on chilling a sample in liquid nitrogen had been noted previously [4], Of two simplified methods of isolating the material without distillation [4,5],... 

McKean, D. C., J. E. Boggs, and L. Schafer. 1984. CH Bond Length Variations Due to the Intramolecular Environment a Comparison of the Results Obtained by the Method of Isolated CH Stretching Frequencies and by Ab Initio Gradient Calculations. J. Mol. Struct. 116, 313-330. 

The ease with which dissolution of the acetylated products can be achieved is affected by the method of isolation. In the author s experience, drying of the acetate with alcohol and ether results in apparent insolubility (even though the product was soluble at one stage of the purification process), and should be avoided. Drying, under diminished pressure, of the product precipitated by petroleum ether is sufficient. Chloroform is probably the best solvent. Nitroethane, tetrachlorethane, 2,4-pentanedione, pyridine, methyl acetate, ethyl acetate, and benzene, which have also been suggested, have disadvantages in that either they are unstable or they may cause aggregation in solution.44,116 116... 

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