Diluted Alcohol

Suspend in a round-bottomed flask 1 g. of the substance in 75-80 ml. of boihng water to which about 0 -5 g. of sodium carbonate crystals have been added, and introduce slowly 4 g. of finely-powdered potassium permanganate. Heat under reflux until the purple colour of the permanganate has disappeared (1-4 hours). Allow the mixture to cool and carefully acidify with dilute sulphuric acid. Heat the mixture under reflux for a further 30 minutes and then cool. Remove any excess of manganese dioxide by the addition of a little sodium bisulphite. Filter the precipitated acid and recrystallise it from a suitable solvent (e.g., benzene, alcohol, dilute alcohol or water). If the acid does not separate from the solution, extract it with ether, benzene or carbon tetrachloride. 

If the presence of a disulphonyl derivative from a primary amine is suspected (e.., formation of a precipitate in alkaline solution even after dilution), reflux the precipitate, obtained after acidifyim , with a solution of I g. of sodium in 20 ml. of rectifled spirit for 15 minutes. Evaporate the alcohol, dilute with water, and filter if necessary acidify with dilute hydrochloric acid. Collect the sulphonyl derivative and recrystallise it from alcohol or dilute alcohol. 

Heat the amine with one or two mols of redistilled benzaldehyde (according as to whether the base is a monamine or diamine) to 100° for 10 minutes if the molecular weight is unknown, use 1 g. of the base and 1 or 2 g. of benzaldehyde. Sometimes a solvent, such as alcohol (5 ml.) or acetic acid, may be used. Recrystallise from alcohol, dilute alcohol or benzene. 

Dissolve 0 -5 g. of the phenol in 4-5 ml. of dry p ridine, add 1 - 3 g. of 3 5-dinitrobenzoyl chloride and reflux for 25-30 minutes. Pour the cold reaction mixture into 40 ml. of ca. 2N hydrochloric acid. Decant the supernatant aqueous hquid from the precipitated sohd or oil and stir it vigorously with about 10 ml. of N sodium carbonate solution. Filter off the sohd derivative and wash it with water. RecrystaUise from alcohol, dilute alcohol, benzene - acetone or benzene - light petroleum (b.p. 60-80 ),... 

Oximes (compare Section III,74,B). The following procedure has wide application. Dissolve 0-5 g. of hydroxylamine hydrochloride in 2 ml. of water, add 2 ml. of 10 per cent, sodium hydroxide solution and 0-2 g. of the aldehyde (or ketone). If the latter is insoluble, add just sufficient alcohol to the mixture to give a clear solution. Heat the mixture under reflux for 10-15 minutes, and then cool in ice. If crystals separate, filter these off, and recrystallise from alcohol, dilute alcohol, benzene or light petroleum (b.p. 60-80°). If no solid separates on cooling, dilute with 2-3 volumes of water, filter the precipitated sohd, and recrystallise. 

Cotton 300 Good resistance to water, alcohol, dilute aqueous solutions. 

Paraformaldehyde (7.5 g) (0.25 mol) and 18.3 g (0.25 mol) of diethylamine are mixed in 25 cc of alcohol and warmed until a clear solution Is obtained. The solution is cooled and mixed with 26.6 g (0.10 mol) of 3,3 -diallyl-4,4 -biphenol in 25 cc of alcohol. After standing several hours, the solution is warmed for one hour on the steam bath, allowing the alcohol to boil off. The residue is then taken up in ether and water, the ether layer separated and washed with 2% sodium hydroxide solution and finally with water. The washed ether solution is dried over solid potassium carbonate, and filtered. After acidifying with alcoholic hydrogen chloride, the ether is distilled off and the alcoholic residue diluted with an equal volume of acetone. The crystalline hydrochloride is filtered off, triturated with alcohol, diluted with several volumes of acetone, filtered and dried MP 209°-210°C. 

Hydrocinnamic acid. Reflux a mixture of 53 5 g. of propiophenone (Section IV,137), 20-6 g. of sulphur and 46 g. (46 ml.) of morpholine for 6 horns. Pour the reaction product into 400 ml. of 10 per cent, alcohohc sodium hydroxide solution and reflux for 7 hours. Distil off the alcohol, dilute with water, acidify with hydrochloric acid (to Congo red paper), and extract three times with ether. Wash the ether extracts with water, dry, remove the ether and distil. Collect the hydrocinnamic acid at 125-129°/ 6 mm. it solidifies completely on cooling, m.p. 46-47°. The yield is 39 g. 

A. Ethyl Nitrite.—Two solutions are prepared. Solution I contains 620 g. (9 moles) of sodium nitrite (650 g. of technical 95 per cent), 210 g. (4.57 moles) of alcohol (285 cc. of 90 per cent denatured, or its equivalent) and water to make a total volume of 2500 cc. Solution II contains 440 g. of sulfuric acid (255 cc. of sp. gr. 1.84) and 210 g. of alcohol, diluted with water to 2500 cc. Ethyl nitrite may he generated cont inuously in gaseous form by allowing solution II to (low into solution I. 

Trinitrobenzene can be prepared by heating w-dinitro-benzene with nitric acid and sulfuric acid to 1200 1 by heating 2, 4, 6-trinitrotoluene with fuming nitric acid in a sealed tube at 180° for three hours 2 by heating 2, 4, 6-trinitrobenzoic acid or its sodium salt with water, alcohol, dilute sodium carbonate or other suitable solvent.3... 

Graded alcohols Dilute 100% alcohol with DEPC-treated water to make 50, 70, and 95% alcohols. 

Eels, Anguilla anguilla, are extremely sensitive to odors. Their detection threshold for /3-phenylethyl alcohol lies at the unbelievable concentration of 3 X 10 mol/l. This corresponds to 1ml of this alcohol diluted in 58 times the volume of Lake Constance (80km long) in southern Germany where these experiments were performed. It has been calculated that only three molecules are in the olfactory sac at any one time (Teichmann, 1957, 1959). Coho salmon... 

N. Schoor] and A. Regenborn say that owing to the ready formation of hydrogen iodide, accurate determinations of the solubility in aq. alcohol can be made only by making a sat. soln. of iodine in absolute alcohol, diluting the soln., and determining the iodine at once. The solubility follows a fairly regular course ... 

Suspend 0 25 g. of 2 4-dinitrophenylhydrazine in 5 ml. of methanol and add 0-4 0-5 ml. of concentrated sulphuric acid cautiously. Filter the warm solution and add a solution of 0-1-0-2 g. of the carbonyl compound in a small volume of methanol or of ether. If no solid separates within 10 minutes, dilute the solution carefully with 2N sulphuric acid. Collect the solid by suction filtration and wash it with a little methanol. ReorystaUise the derivative from alcohol, dilute alcohol, alcohol with ethyl acetate or chloroform or acetone, acetic acid, dioxan, nitromethane, nitrobenzene or xylene. 

Decolorizing Power. — Dissolve 50 gm. of caramel (sugar coloring burnt sugar) in 50 cc. of water, add 100 cc. of 85 per cent alcohol, dilute the whole to 1 liter, allow to stand for several days, and then filter. Dilute 5 cc. of this caramel solution with 50 cc. of water, add 1 gm. of animal charcoal, boil the mixture ten minutes under a reflux condenser, and then filter. The filtrate should be perfectly colorless. 

A very reactive sodium ethylate can be obtained by adding the calculated quantity of absolute alcohol diluted with 2 vols. of dry xylene to granulated sodium under xylene (see below). During the addition the whole is well cooled and shaken. The xylene is then distilled off in a current of dry hydrogen. 

Standard solution Transfer about 50 mg of USP Omeprazole RS, accurately weighed, to a 250-ml volumetric flask, dissolve in 50 ml of alcohol, dilute with 0.01 M sodium borate solution to volume, and mix. Transfer 10 ml of this solution into a 100-ml volumetric flask, add 20 ml of alcohol, dilute with 0.01 M sodium borate solution to volume, and mix. 

Fig. 19. Lightscattering data for AOT in t-amyl alcohol (square points) and in t-amyl alcohol diluted with nonane (round points). Open and solid points represent Hg-green and blue line data, respectively. [J. Colloid Interface Sci. 29, 6 (1969)]...

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