Methanol nitration

Nitromethoxy methanol nitrate produced a lead block expansion of 420 cm whereas the net expansion produced by nitroglycol in the same series of experiments was 450 cm3. 

Citric Acid Method (CA) Ce and Zr nitrate (Ce(N03)3 6H20 and Zr0(N03)2 6H20) precursors were dissolved in methanol (ratio of methanol/nitrate solution = 2 1 (v/v)) and excess citric acid was added (molar ratio of N03 /acid = 6 1.15). The resulting solution was stirred at room temperature for at least 12 hours. The solvent and the reaction products were eliminated using a rotary evaporator at room temperature. The most important step in... 

Nitromethoxy methanol nitrate, also called methyl ether nitro nitrate, is a colorless oily liquid with slightly higher explosion property than glycol dinitrate. It is a liquid explosive with a wide application potential. 

Properties of nitromethoxy methanol nitrate Molecular formula C2H4O6N2 Chemical structure ... 

Its shock sensitivity is stronger than glycol dinitrate. It has been found that 10 % explosion risk for glycol dinitrate needs shock energy of 0.91 kg m/cm, while for nitromethoxy methanol nitrate only 0.11 kg m/cm is needed. Nitromethoxy methanol nitrate is able to dissolve collodion and more volatile than glycol nitrate. The chemical stability and explosion property of nitromethoxy methanol nitrate and its cellulose nitrate solution are weak. 

The lead-block value of nitromethoxy methanol nitrate is 420 cm. In the same conditions, the value of glycol dinitrate is 450 cm. Nitromethoxy methanol nitrate has similar explosion property and low chemical stability. Its shock sensitivity is high and the lead-block value is 440 cm. ... 

Nitromethoxy methanol nitrate can be prepared by nitration reaction of bis-chloromethyl ether. Bis-chloromethyl ether can be obtained by the following reaction between 40 % formaldehyde solution and hydrogen chloride gas ... 

In the reaction, chlorine ether of CICH2OCH2OCH2CI is formed. The chlorine ether will be converted to another nitrate ester, O2NOCH2-O-CH2OCH2NO2, with boiling point of 88 °C (9 mmHg) in the later nitration reaction. Nitromethoxy methanol nitrate is more volatile than glycol nitrate, but less than other nitro nitrate esters. 

Analytical Procedures. Standard methods for analysis of food-grade adipic acid are described ia the Food Chemicals Codex (see Refs, ia Table 8). Classical methods are used for assay (titration), trace metals (As, heavy metals as Pb), and total ash. Water is determined by Kad-Fisher titration of a methanol solution of the acid. Determination of color ia methanol solution (APHA, Hazen equivalent, max. 10), as well as iron and other metals, are also described elsewhere (175). Other analyses frequendy are required for resia-grade acid. For example, hydrolyzable nitrogen (NH, amides, nitriles, etc) is determined by distillation of ammonia from an alkaline solution. Reducible nitrogen (nitrates and nitroorganics) may then be determined by adding DeVarda s alloy and continuing the distillation. Hydrocarbon oil contaminants may be determined by ir analysis of halocarbon extracts of alkaline solutions of the acid. 

Isoprene [78-79-5] (2-methyl-1,3-butadiene) is a colorless, volatile Hquid that is soluble in most hydrocarbons but is practically insoluble in water. Isoprene forms binary azeotropes with water, methanol, methylamine, acetonitrile, methyl formate, bromoethane, ethyl alcohol, methyl sulfide, acetone, propylene oxide, ethyl formate, isopropyl nitrate, methyla1 (dimethoxymethane), ethyl ether, and / -pentane. Ternary azeotropes form with water—acetone, water—acetonitrile, and methyl formate—ethyl bromide (8). Typical properties of isoprene are Hsted in Table 1. 

Compounds of type (42) are widely used in the dye industry (see Azo dyes). The Mannich reaction also takes place at C, as does halogenation and nitration. The important analgesic aminoantipyrine [83-07-8] (43) on photolysis in methanol undergoes ring fission to yield (44) (27). 

Nitrobenzotrichloride is also obtained in high yield with no significant hydrolysis when nitration with a mixture of nitric and sulfuric acids is carried out below 30°C (31). 2,4-Dihydroxybenzophenone [131 -56-6] is formed in 90% yield by the uncatalyzed reaction of benzotrichloride with resorcinol in hydroxyHc solvents (32) or in benzene containing methanol or ethanol (33). Benzophenone derivatives are formed from a variety of aromatic compounds by reaction with benzotrichloride in aqueous or alcohoHc hydrofluoric acid (34). 

The side-chain chlorine contents of benzyl chloride, benzal chloride, and benzotrichlorides are determined by hydrolysis with methanolic sodium hydroxide followed by titration with silver nitrate. Total chlorine determination, including ring chlorine, is made by standard combustion methods (55). Several procedures for the gas chromatographic analysis of chlorotoluene mixtures have been described (56,57). Proton and nuclear magnetic resonance shifts, characteristic iafrared absorption bands, and principal mass spectral peaks have been summarized including sources of reference spectra (58). Procedures for measuring trace benzyl chloride ia air (59) and ia water (60) have been described. 

Cyclohexanoae is miscible with methanol, ethanol, acetone, benzene, / -hexane, nitrobenzene, diethyl ether, naphtha, xylene, ethylene glycol, isoamyl acetate, diethylamine, and most organic solvents. This ketone dissolves cellulose nitrate, acetate, and ethers, vinyl resias, raw mbber, waxes, fats, shellac, basic dyes, oils, latex, bitumea, kaure, elemi, and many other organic compounds. 

Cerium(IV) ammonium nitrate in methanol has been used to oxidize phenazine to the mono-N-oxide (41) in good yield (75JCS(P1)1398), but no other reports on the application of this reagent to the pyrazine or quinoxaline series have appeared. 

To a solution of 33 g. (O.S mole) of potassium hydroxide (Note 1) in 1.5 1. of distilled water in a 5-1. flask or other appropriate container fitted with a mechanical stirrer is added 80 g. (0.5 mole) of methyl hydrogen adipate (Note 2). With continuous stirring a solution of 85 g. (0.5 mole) of silver nitrate in 1 1. of distilled water is added rapidly (about IS minutes). The precipitated methyl silver adipate is collected on a Buchner funnel, washed with methanol, and dried in an oven at 50-60°. For the next step the dried silver salt is finely powdered and sieved through a 40-mesh screen. The combined yield from two such runs is, 213 g. (80%). 

Ammonium nitrate and other ammonium salts Any oxidizable substance, such as ethanol, methanol, glacial acetic acid, acetic anhydride, benzaldehyde, carbon disulphide, glycerol, ethylene glycol, ethyl acetate, methyl acetate or furfural Chlorates, perchlorates, permanganates... 

E] silica smoke Sod.Nit.Prus. n Sod.Nitrate <0 Sod. Sulphite m Methanol (D) n water... 

Silver cyanate should be freshly prepared. The commercial material has a pronounced gray color and is totally unsuitable for this reaction. Best results are obtained when the following preparation is carried out in the dark. To 100 g of silver nitrate in 3 liters of distilled water is added with stirring 49.5 g of potassium cyanate in 700 ml of distilled water. The white precipitate is filtered through a large Buchner funnel (Coors No. 5) and the filter cake is washed with 500 ml water, then with 300 ml methanol, and finally with... 

Treatment of dibromocarbene adduct (43) (Rji, = O) with aqueous methanol containing silver nitrate or perchlorate gives A-homo-estra-1 (10), 2,4a-triene-4,17-dione (45) in 21 % overall yield from the enol ether (42). The exact pathway is not known, but the first step may be formation of a bromo-homo-dienone facilitated by the methoxyl group, which then undergoes further loss of hydrogen bromide involving shift of a double bond by enolization. ... 

Commercial grades of PVP, K-15, K-30, K-90, and K-120 and the quaternized copolymer of vinylpyrrolidone and dimthylaminoethylmethacrylate (poly-VP/ DMAEMA) made by International Specialty Products (ISP) were used in this study. PEO standard calibration kits were purchased from Polymer Laboratories Ltd. (PL), American Polymer Standards Corporation (APSC), Polymer Standards Service (PSS), and Tosoh Corporation (TSK). In addition, two narrow NIST standards, 1923 and 1924, were used to evaluate commercial PEO standards. Deionized, filtered water, and high-performance liquid chromatography grade methanol purchased from Aldrich or Fischer Scientific were used in this study. Lithium nitrate (LiN03) from Aldrich was the salt added to the mobile phases to control for polyelectrolyte effects. 

Solvent can affect separation in two different ways. Because water is a better solvent for these four columns than water/methanol, based on the swelling or void volume of the columns in Table 17.9, the separation should be better in water than in water/methanol. The relative viscosity of a 0.5% PEO standard from Aldrich (Lot No. 0021kz, MW 100,000) in water and in water/methanol with 0.1 M lithium nitrate is 1.645 and 1.713, respectively. This indicates that the hydrodynamic volume of PEO in water is smaller than in water/methanol. The difference in hydrodynamic volume between two PEO standards should also be larger in water/methanol than in water. Hence, the separation for PEO should be better in water/methanol than in water. The results in Table 17.8 indicate that separation efficiency is better in water than in water/methanol... 

In summary, methanol as a mobile-phase modifier has a significant effect on the separation of PVP in aqueous SEC with these four linear columns. The best separation of all PVP grades can be achieved with the SB-806M column in 50 50 water/methanol with 0.1 M lithium nitrate. It is interesting to note that despite the improvements reported by the manufacturers for the newer columns (SB-806MHQ and PWxl), the newer columns do not necessarily perform better than the older columns (SB-806 and PW) for aqueous SEC of PVP. 

A three-necked round-bottom flask is fitted with a dropping funnel, a thermometer, and a magnetic stirrer and is heated in a water bath to 30°. Tetralin (1.32 g, 0.01 mole) and 50 ml of 3.5 Anitric acid solution are placed in the flask and brought to temperature. Ceric ammonium nitrate (21.9 g, 0.04 mole) is dissolved in 100 ml of 3.5 N nitric acid, and the solution is added dropwise to the reaction mixture at a rate such that the temperature does not rise and only a pale yellow color is evident in the reaction mixture. At the completion of the reaction (1 to 2 hours), the mixture should be colorless. The solution is cooled to room temperature, diluted with an equal volume of water, and extracted twice with ether. The ether solution is dried with anhydrous sodium sulfate, filtered, and the ether is evaporated. The residue may be distilled to yield a-tetralone (bp 113-11676 mm or 170749 mm) or may be converted directly to the oxime, which is recrystallized from methanol, mp 88-89°. 

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