Impurities, in methanol

A new mechanism, called the methane-formaldehyde mechanism, has been put forward for the transformation of the equilibrium mixture of methanol and dimethyl ether, that is, for the formation of the first C-C bond.643 This, actually, is a modification of the carbocation mechanism that suggested the formation of ethanol by methanol attaching to the incipient carbocation CH3+ from surface methoxy.460,462 This mechanism (Scheme 3.3) is consistent with experimental observations and indicates that methane is not a byproduct and ethanol is the initial product in the first C-C bond formation. Trimethyloxonium ion, proposed to be an intermediate in the formation of ethyl methyl ether,447 was proposed to be excluded as an intermediate for the C-C bond formation.641 The suggested role of impurities in methanol as the reason for ethylene formation is highly speculative and unsubstantiated. 

Reagent grade methanol must be used because trace impurities in methanol can increase the conductivity of transfer buffer and decrease transfer efficiency. 

Methanol. Traces of metallic impurities in methanol can lead to an explosion and ignition of the methanol on introduction of chlorine.23... 

In Figure 3, plots of absorbance for three combinations of water and methanol of various purity are shown. The main sovuce of UV absorption of the binary mobile phase was evidently the impurities in methanol. A comparison of both the bottom curves shown in Figure 3 also proves the effectiveness of water purification by distillation. 

Figure 11.20 (a) Effect of RR and solvent on methanol purity with chlorobenzene solvent, (b) Effect of RR and solvent on impurities in methanol product with chlorobenzene solvent. 

The alcoholysis reaction may be carried out either batchwise or continuously by treating the triglyceride with an excess of methanol for 30—60 min in a well-agitated reactor. The reactants are then allowed to settle and the glycerol [56-81-5] is recovered in methanol solution in the lower layer. The sodium methoxide and excess methanol are removed from the methyl ester, which then maybe fed directiy to the hydrogenolysis process. Alternatively, the ester may be distilled to remove unreacted material and other impurities, or fractionated into different cuts. Practionation of either the methyl ester or of the product following hydrogenolysis provides alcohols that have narrow carbon-chain distributions. 

The quahty of formamide suppHed by BASE is certified as having a minimum assay of 99.5%. The principal impurities in the material are ammonium formate, methanol, water, and traces of iron. The quaUty of formamide supphed by BASE is certified to meet the specifications given in Table 3. 

The impure product is dissolved in methanol. Subsequent reaction with ammonium fluoride forms ammonium hexafluorotitanate. This soHd, obtained in high purity, reacts with water vapor in a stream of air at 250°C to give anatase. 

Diels and Meyer found that the exothermic reaction obtained on dropping pyridine into dimethyl acetylenedicarboxylate in methanol gave a mixture of the indolizine (108) and a methoxymethylindolizine formulated as (109), and some dimethyl fumarate and dimethyl methoxyfumarate. Later workers - obtained only the methoxymethylindolizine in rather poor yield. The indolizine (108) has also been isolated from the products obtained when the addition reaction was carried out in ether, but in this case the course of the reaction was very susceptible to the presence of impurities in the ether, and the results indicated that ethanol was necessary as a reactant. ... 

Arylpentazoles can be prepared by adding an aqueous solution of azide to a mixture of an aryldiazonium chloride, aqueous methanol, and petroleum ether at —40 to —20° with stirring. The pure aryl-pentazole (see Table I) crystallizes from the two-phase reaction mixture the inorganic impurities remain in the aqueous methanol and the organic impurities in the petroleum ether. 

A mixture of 26.1 g of o-benzylphenoxy- J-chloropropane and 17 g of pipiridine Is refluxed over a period of 32 hours until the temperature is about 124t and a nearly solid mixture is formed due to the precipitation of a salt. The mixture is then refluxed over a period of 48 hours at about 160 3 and the reaction product obtained is cooled and dissolved in methanol. The solution is concentrated under reduced pressure to yield an oil which is added to 200 ml 3N hydrochloric acid whereupon the mixture is shaken with ether, 3 x 100 ml, until the aqueous phase Is clear. The ether solution is washed with water, 3 x 50 ml, and the water present in the combined aqueous phase and water used for washing Is evaporated under reduced pressure methanol being added three times when the residue appears to be dry. The impure hydrochloride of o-benzylphenoxy- J-N-piperidinopropane, 41 g, obtained is dissolved in 100 ml water and 100 ml 30% aqueous sodium hydroxide solution are added, whereupon precipitated oil is extracted with ether, 1 x 100 and 2 x 50 ml. The ether solution is washed with water, 4 x 50 ml, dried with magnesium sulfate and the ether is removed under reduced pressure. The residue, 252 g, is distilled under reduced pressure and the main fraction,... 

Impurities in other solvents may affect chromatographic behaviour, or detection, or both. Chlorinated solvents such as di- or trichloromethane are stabilised against oxidative breakdown by the addition of small amounts of methanol or ethanol. 

Figure 2. Auger electron spectrum of the surface of two Ru electrodes after deactivation by reduction of carbon monoxide and methanol at higher temperatures (75 and 90 °C respectively in 0.2 M Na2SC>4 at pH 4 and -0.545 V vs SCE ). The presence of K on the surface must result from the adsorption of K+ ions present as an impurity in the electrolyte.

The iron present as an impurity in silica gel-G affords an appreciable distortion of the chromatogram . Hence, it has become almost a necessary step to purify the adsorbent. The iron-free layers may be achieved by providing the pre-coated and air-dried plates a preliminary development with a mixture of methanol and... 

Nbdifying the platinum surface with Nafion enhanced the sustained ciurent. This effects appeared to stem from the protection effect from impurities. Supplying methanol fit>m the gas phase did not show much differoice in the methanol oxidation characteristics from supplying it 6rom the electrolyte phase. 

FIGURE 1.25 HPLC determination of impurities in a levothyroxin (L-T4) formulation. Experimental conditions Column, Chiralpak QN-AX (150 rum x 4 rum ID) mobile phase, acetonitrile-50 mM ammonium acetate (60 40, v/v) (pHa 4.5) flow rate, 0.7 mLmiu UV detection, 240 nm temperature, 25 C. Sample, T4-200 tablets (Uni-Pharma, Greece) containing 0.2 mg L-T4 sodium per tablet the tablet was pulverized, suspended in methanol-10 mM sodium hydroxide (1 1 v/v) and after ultrasonication for 5 min the residues were removed by filtration. An aliquot of 10 xL of the filtrate was directly injected. (Reproduced from H. Gika et al., J. Chromatogr. B, 800 193 (2004). With permission.)... 

Note Impurities in commercially available nitromethane identified by GLC include 1-nitro-propane, 2-nitropropane, acetaldehyde, acetonitrile, methanol, ethanol. In addition, formaldehyde, ethyl acetate, and acetone may be present (Jarosiewicz and Szychlinski, 1980)... 

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