Ethanol dilute

The hydrolysis of as little as 0 5 ml. of the ester can be carried out in the combined reflux-distillation apparatus shown in Fig. 38 (p, 63). Pass a stream of cold water through the vertical condenser. Place in the 10 ml. pear-shaped flask 0 5 ml. of the ester, 5 ml. of 10% NaOH solution and one or two minute fragments of unglazed porcelain and heat the mixture gently for 15 minutes so that the vapours do not rise more than about half-way up the vertical water ondenser. Now run the water out of the ver ical condenser, insert a thermometer at the top, and pass water through the inclined condenser. Heat the flask sufficiently strongly to collect 1--2 ml. of distillate. This is dilute ethanol. 

Place 1 0 ml. of hydrazine hydrate (CAUTION corrosive chemical) in a test-tube fitted with a short refiux condenser. Add 10 g. of the methyl or ethyl ester dropwise (or portionwise) and heat the mixture gently under refiux for 15 minutes. Then add just enough absolute ethanol through the condenser to produce a clear solution, refiux for a further 2-3 hours, distil oflF the ethyl alcohol, and cool. Filter oflF the crystals of the acid hydrazide, and recrystallise from ethanol, dilute ethanol or from water. 

The sulphonanilldes may be prepared by either of the following methods —(i) Reflux the solution of the sulphonyl chloride in benzene obtained as above, with 2 5 g. of aniline for 1 hour. Concentrate the benzene solution to half its volume and cool in ice. Collect the solid which separates on a filter, wash with hot water, and recrystallise from ethanol or dilute ethanol. 

Dissolve 1 g. of the sulphonic acid or its sodium salt in the minimum volume of boiling water and add a saturated aqueous solution of 1 g. of p-toluidine hydrochloride. Cool, Alter off the precipitate of the p-tolu-idine salt, and recrystallise it from hot water or from dilute ethanol. 

A simplified procedure is possible by using polyphosphoric acid as the condensing agent. Add 160 g. of polyphosphoric acid to a solution of 11 g. of resorcinol in 13 g. of ethyl acetoacetate. Stir the mixture and heat at 75-80° for 20 minutes, and then pour into ice-water. Collect the pale yellow solid by suction filtration, wash with a little cold water, and dry at 60°. The yield of crude 4-methyl-7-hydroxycoumarin, m.p. 178-181°, is 17 g. Recrystalbsation from dilute ethanol yields the pure, colourless compound, m.p. 185°. 

To a solution of 50 grams of 6,7-dimethoxy-3-methyl-T(4 -ethoxy-3 -methoxybenzyl)-dihy-droisoquinoline base in 200 ml of dry benzene are added 150 ml of decalin, and the mixture is distilled until its temperature reaches 180°C. 1.5 grams of 5% palladium on carbon are then added. The mixture is stirred under reflux for about 6 hours to dehydrogenate the dihydroisoquinoline. On cooling, the reaction mixture is diluted with petroleum ether and the precipitated 6,7-dimethoxy-3-methyl-1-(3 -methoxy-4 -ethoxybenzyl)-isoquinoline is filtered off and recrystallized from dilute ethanol. 

The combined ether extracts were washed with 5% aqueous sodium bicarbonate solution, dried over anhydrous sodium sulfate, and fractionally distilled in vacuo. The fraction boiling at about 145° to 150°C at the pressure of 0.5 mm of mercury, weighing 61 g and consisting of 1-methyl-5-allyl-5-(1-methyl-2-pentynyl) barbituric acid, was collected. The only distillate was substantially pure, and could be used as such In pharmaceutical preparation or a salt could be prepared therefrom according to the procedures disclosed hereinafter. On standing, the oil crystallized. The crystalline 1-methyl-5-allyl-5-( 1-methyl-2-pentynyl) barbituric acid melted at about 60° to 64°C after recrystallization from dilute ethanol. 

Preparation of Diethylphenylacetic Acid 46 grams of the foregoing nitrile was added to 140 ml ethylene glycol containing 36 grams potassium hydroxide and the mixture refluxed with stirring for about 20 hours. The mixture was diluted with water, extracted with light petroleum (8P 60° to 80°C) to remove traces of impurities and then acidified to yield diethylphenylacetic acid which was recrystallized from dilute ethanol (40% v/v ethanol in water). 

Pipethanate hydrochloride Is dissolved in water and the solution is made alkaline by adding 10% sodium hydroxide solution. The crystals that are separated are filtered off and recrystallized from dilute ethanol. The monohydrate thereby obtained is dehydrated at 100°C under reduced pressure for 20 minutes. The products that are now in the form of a syrup due to loss of water of crystallization are further dehydrated for 2 days in a desiccator over phosphorus pentoxide whereupon the anhydrous pipethanate is obtained. 

Alternative (Bl 3.6 grams (0,01 mol) prednisolone and 4.32 grams (0.012 mol) stearoyl-glycolyl-chloride, separately dissolved in dry dioxane, are added with 0.B9 ml (0.011 mol) dry pyridine. The mixture is kept at 60°C for 20 hours, then poured into water-ice and filtered. Crystallization from diluted ethanol results in prednisolone-21-stearoyl-glycolate (MP 104°-105°C). 

Dimethylglyoxime is almost insoluble in water, and is added in the form of a 1 per cent solution in 90% ethanol (rectified spirit) or absolute ethanol 1 mL of this solution is sufficient for the precipitation of 0.0025 g of nickel. As already pointed out, the reagent is added to a hot feebly acid solution of a nickel salt, and the solution is then rendered faintly ammoniacal. This procedure gives a more easily filterable precipitate than does direct precipitation from cold or from ammoniacal solutions. Only a slight excess of the reagent should be used, since dimethylglyoxime is not very soluble in water or in very dilute ethanol and may precipitate if a very large excess is added (such that the alcohol content of the solution exceeds 50 per cent), some of the precipitate may dissolve. 

If the solution is appreciably colored it may be treated with decolorizing carbon at this point. Toluene or dilute ethanol may also be used for the recrystallization, but these solvents are less satisfactory. 

Recrystallization from dilute ethanol affords colorless material, m.p. 94-95°. 

C. 10 g (II) and 15 g SOCI2 are refluxed on water bath two hours and evaporated in vacuum on water bath. Pour residue into cold liquid NH3 or NH4OH with stirring. Filter, wash precipitate with water to get about 80% yield substituted hydrocinnamamide (III) (recrystallize-benzene or dilute ethanol). 

Biological oxidation of methanol and ethanol in the body produces the corresponding aldehyde followed by the acid. At times the alcoholics, by mistake, drink ethanol, mixed with methanol also called denatured alcohol. In the body, methanol is oxidised first to methanal and then to methanoic acid, which may cause blindness and death. A methanol poisoned patient is treated by giving intravenous infusions of diluted ethanol. The enz5mie responsible for oxidation of aldehyde (HCHO) to acid is swamped allowing time for kidneys to excrete methanol. 

Methoxy-2-Naphthol. A mixture of 10 g of 6-bromo-2-methoxynaphalene, 0.5 g of copper bronze, 8.5 g of NaOH, and 175 cc of water are shaken in a suitable high pressure vessel at 200° for 75 minute. Cool, dilute with a little water, filter copper off, and acidify with coned HCl acid. Collect the resulting product, wash with water and dry in air. Recrystallize the resulting crude product with dilute ethanol to get a little over 5 g. 

DETAILS - Colchicine is a plant drug used in the treatment of gout. It is a very efficient poison in view of its very low toxic dose and the fact that an autopsy will show only the symptoms of acute gastroenteritis. This does not, however, mean it is undetectable. It only means that it is likely to be overlooked. It is also very useful as a dart poison, especially when nicotine is used as a binder. Colchicine is great for small caliber (,22)bullets, as they usually won t hold enough of most other poisons to do any good. It dissolves slowly in water, but faster in dilute ethanol (liquor). As with any plant alkaloid, it is best to harvest the... 

Ethanol, 95% (or industrial methylated spirits, 95%) - dilute ethanol (or IMS) to give 95% v/v ethanol/water. 

Yong and Beng [180] have deposited monolayers of 2-mercaptobenzothiazole and 2-mercaptobenzimidazole on Au surfaces from diluted ethanolic solutions and have studied their electrochemical behavior. 

The procedure described is essentially that of Japp and Klingemann.3 Methylglyoxal-u-phenylhydrazone may also be prepared by heating phenylazoacetoacetic acid at 170-180° 9 or by warming ethyl phenylazoacetoacetate with a solution of sodium hydroxide in dilute ethanol. 8 9... 

Reaction of Ethylenediamine. Using 0.015 mole of diamine, 0.9 gram (61%) of bisacetylacetoneethylenediiminocopper(II) was obtained. Red platelets, m.p. 138-41° (dilute ethanol). There was no depression of melting point on admixture with authentic sample. Using 0.005 or 0.01 mole of amine, a mixture of blue and gray crystals was obtained, suggesting hydrolysis and, certainly, the absence of amine exchange. 

Filter off the crystals on a Buchner funnel, wash them with a small amount of ice-cold water, then with dilute ethanol, and, finally, with a 96% ethanol solution. Write the equations of the reactions. Dry the salt in the air and weigh it. Calculate the yield in per cent. Prove that you have obtained a complex cobalt salt. 

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