Acetic acid ethers

Although no chemical reaction occurs, measurements of the freezing point and infra-red spectra show that nitric acid forms i i molecular complexes with acetic acid , ether and dioxan. In contrast, the infrared spectrum of nitric acid in chloroform and carbon tetrachloride - is very similar to that of nitric acid vapour, showing that in these cases a close association with the solvent does not occur. 

The following general procedure has been used for the reduction of the tosylhydrazone derivatives of various steroidal ketones. A mixture of the tosylhydrazone (50 mg) and sodium borodeuteride (50 mg) in dry dioxane (3 ml) is heated under reflux for 2 hr, and then the excess deuteride is decomposed by the addition of a few drops of acetic acid. Ether is added and the resulting solution is washed with 2 N sodium bicarbonate solution and... 

Procedures have been worked out which increased the yield of 2-bromothiophene to 78% on direct bromination in acetic acid-ether mixtures and to 67% in carbon tetraehlorided With the mild brominating agent, dioxane dibromide, quantitative yields of 2-bromothiophene are obtained. A very convenient procedure for the iodination of thiophenes consists of the acid-catalyzed (HzSOi) reaction with iodine and HIO3, giving 2-iodothiophene in 75% yieldd In contrast to the HgO method, all the iodine is utilized. 

Soluble in acetic acid, ether, ligroin (Weast, 1986), and very soluble in many chlorinated solvents including chloroform, carbon tetrachloride, etc. 

Soluble in acetone, benzene (Weast, 1986), glacial acetic acid, ether (Windholz et al., 1983), and toluene... 

The solvents 1, ethyl acetate-2-propanol-water (126 70 35) 2, 2-propanol-water (90 10) 3, benzene-methanol (10 3) 4, chloroform-acetone (1 7) 5, 1-butanol-acetic acid-ether-water (0 6 3 1) 6, chloroform-2,2,4-trimethylpentane-methanol (50 15 5) 7, chloroform-methanol (10 2). 

The solvents most commonly employed are water, alcohol, ether, benzene, petroleum ether, acetone, glacial acetic acid or mixtures of water and alcohol, water and acetic acid, ether and petroleum ether, benzene and petroleum ether. 

Ethyl acetic acid ether was treated with hydroxylamine and acetohydroxamic acid was obtained. 

Usually o.v-dccalin is formed more selectively from tetralin than from naphthalene. Baker and Schuetz obtained a mixture of 77% cis- and 23% frans-decalin in the hydrogenation of naphthalene over Adams platinum oxide in acetic acid-ether at 25°C and 12.8 MPa H2, while cA-decalin was obtained exclusively in the hydrogenation of tetralin in acetic acid under similar conditions.23... 

N. A. E. Millon found iodic acid to be insoluble in absolute alcohol, but 87 per cent, alcohol dissolves almost half its weight of iodic acid the acid is also insoluble in acetic acid, ether, chloroform, carbon disulphide, and in hydrocarbons. 

Di-(hydroxy acetic acid) ether Di-glycolic acid... 

Ethyl ether and ethyl ester of hydroxy acetic acid Ether-ester)... 

The distillate contains ethyl acetate, and small amounts of alcohol, acetic acid, ether, water, and sulfur dioxide. Transfer the distillate into a separatory funnel, and add small amounts of a saturated solution of sodium carbonate until the upper layer is no longer acid (test with litmus). Remove the lower aqueous layer. The remaining layer contains the ester and a small amount of ethanol. Shake with 10 ml of concentrated calcium chloride solution to remove traces of alcohol. Dry the ester with 6 g of anhydrous magnesium sulfate, then transfer to a distilling flask and fractionate. The portion which boils below 73° is rejected. The fraction boiling at 73-80° is collected. The yield is about 40-50 g. 

Silica gel G Toluene-acetic acid-ether methanol (120 18 60 1) FeCI3 spray reagent 75... 

Stable for convenient manipulation. For these reasons /-butyl azidoformate is used widely in peptide synthesis. The group is stable to hydrogenation and to sodium in liquid ammonia and is more resistant to alkali than the carbobenzoxy group. It is readily removed by hydrogen bromide in acetic acid. Selective removal of this group in the presence of a carbobenzoxy group can be accomplished with hydrogen chloride in acetic acid, ether, ethyl acetate, or nitromethane. 

A suspension of anhydrous silver acetate in boiling acetic acid is then added. After the mixture is stirred for 1 minute, the supernatant is again decanted and the black zinc-silver couple is washed with acetic acid, ether and finally methanol. Some of the results they obtained are shown in Table 8. 

Kieselgel G Methanol acetic acid ether benzene (1 9 30 60) 86... 

Properties White crystals aromatic odor and taste. D 0.979, mp 48-51, bp 233C. Soluble in alcohol, carbon disulfide, chloroform, glacial acetic acid, ether, and fixed or volatile oils slightly soluble in water and glycerol. Combustible. 

Carbamates. /3-Iodocarbamates can be reduced to carbamates by refluxing with powdered zinc in 1 1 acetic acid-ether for 5-24 hours. Yields are in the... 

As examples the separation of aspirin, caffeine, and phenacetin (APC tablets) is accomplished by a mobile phase of methanol-acetic acid-ether-benzene (1 18 60 120) and nitroglycerine, a vasodilator, present in heart medication capsules can be separated from the other capsule materials by benzene. 

Extraction of water from an aqueous solution of alcohols, separation of benzene/cyclohexane mixtures Extraction of ethanol from an aqueous solution Extraction of ethanol from an aqueous solution Extraction of ethanol from an aqueous solution Extraction of water from an aqueous solution of alcohols, acetic acid, ethers, pyridine, etc. 

Plates from hot benzene + methanol, rop 206 -206.5. [n) J —36,3 (c = 3.8 in ethanol), uv max (ethanol) 223, 272, 304.5 nm (< 11,300 6350 5100). Sol in ethanol, methanol, dioxane, acetone, pyridine, coned HjSO( moderately sol in acetic acid, ether sparingly sol in benzene, petr ether, chloroform, water. Gives yellow solns with aq ammonia, sodium carbonate, and sodium hydroxide. Alkaline solns darken rapidly in air, eventually becoming purple. 

Coral-like clusters from pyridine + acetone, mp 230-240 with sintering at 180-190. [ ]Jf —10.8 (c = 2 in pyridine). Practically insol in water, cold methanol, acetone, cold acetic acid, ether, acetonitrile. Soluble in pyridine, chloroform, hot methanol, hot acetic acid. Dissolves readily in chloroform + methanol mixtures of high chloroform content. 

Yellow needles from ale, mp 312° (dec). Sublimes above 310°. Moderately sol in boiling nitrobenzene sparingly sol in boiling ale. somewhat more sol in a mixture of glacial acetic acid and nitric acid. Practically insol in acetone, chloroform, benzene, dioxane. acetic acid, ether and linseed Oil-Solubilities in g/100 ml solvent at 25° watet 2 x I0 ethanol 0.007 ethyl acetate 0.015 petr ether 0.0 xylene <0.01 methyl Cellosolve 0.1 dimethyl acetamide 0.14 dimethyl sulfoxide 0.47. 

Orange-COlored, diamond-shaped plates from ale, mp 230°. uv max 355, 283 nm (e 27,600 1000). Practically insol in water, petr ether. Sol in chloroform, acetone, ethyl acetate, acetic acid, ether, benzene. Slightly sol in cold etha -nol, more so] in hot ethanol. Dissolves in aq solns of alkali hydroxides and pyridine with an intense purple color. Easily reduced by hydrosulfite or other reducing agents to the col -orless dihydrofuscin, C.sH 0 , mp 206. which is also found in the metabolic soln from the fungus grown on Czapek-Dox medium. 

White crystalline powder from boiling water, mp 135-140". Partly sol in water, acetic acid, ether sol in alcohol, pyridine. Practically insol in hydrocarbons and chloroform. THERAP CAT Anxiolytic. 

The products of addition of bromine to unsaturated steroids play a part, as intermediates, in steroid rearrangements. The reaction is carried out in glacial acetic acid, ether, or chloroform at temperatures below 20° and leads... 

CH2C12, CHC13, and CC14 can be used as solvents for addition of HI at room temperature, and also for that of HC1 or HBr for the last two, benzene, toluene, xylene, nitrobenzene, light petroleum, hexane, heptane, nitromethane, glacial acetic acid, ether, and dioxan can also be used, but ether and dioxan decelerate ionic addition. 

From the aromatic ether wtth bromine in alcohol, acetic acid, ether, chloroform or petrol ether See Wild, pp 98-9, 101, H W Underwood, O L BanI and G C Toone, J Amer Chem Soc, 52, 4087 (1930)... 

You will see on the walls the well-known acetylene tree diagram. This shows the wide range of products that can be made from calcium carbide and are made elsewhere - alas, not here - alcohol, acetaldehyde, acetic acid, ether, acetone, ethylene, the vinyl products, solvents, plastics, artificial silk, resins, rubbers. .. Calcium carbide is the only substance which provides these indispensable commodities without requiring one ton of shipping. It is the only route by which they can be made without adding a penny to our already unfavourable balance of trade. It is the only material which costs neither blood nor treasure in war time. .. Our imports of calcium carbide were last year about 70,000 tons. They are increasing. ... 

Properties Colorless cryst. sol. in 95% ethanol, CS2, acetic acid, ether, benzene insol. in water ... 

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