Water reaction with hydrochloric acid

Into a 500 nil. round-bottomed flask, provided with a double surface condenser, place 50 g. (63 ml.) of pure, dry acetone, 50 g. (47 ml.) of ethyl cyanoacetate (Section 111,131) and 0 -5 g. of piperidine. Allow to stand for 60 hours and heat on a water bath for 2 hours. Treat the cold reaction mixture with 100 ml. of ether, wash with dilute hydrochloric acid, then with water, and dry over anhydrous sodium or magnesium sulphate. Distil under diminished pressure and collect the ethyl fsopropylidene cyanoacetate (ethyl a-cyano-pp-dimethylacrylate) at 114-116°/14mm.(l). The yield is 39 g. 

In an alternative procedure 26 g. of anhydrous ferric chloride replace the aluniiniuni chloride, the mixture is cooled to 10°, and the 50 g. of tert.-butyl chloride is added. The mixture is slowly warmed to 25° and maintained at this temperature until no more hydrogen chloride is evolved. The reaction mixture is then washed with dilute hydrochloric acid and with water, dried and fractionally distilled. The yield of tert.-butyl benzene, b.p. 167- 170°, is 60 g. 

Into a stirred, cooled (10°-15°C) solution of 26.2 grams (0.1 mol) of 2-amino-5-chlorobenzo-phenone (3-oxime in 150 ml of dioxane were introduced in small portions 12.4 grams (0.11 mol) of chloracetyl chloride and an equivalent amount of 3 N sodium hydroxide. The chlor acetyl chloride and sodium hydroxide were introduced alternately at such a rate so as to keep the temperature below 15°C and the mixture neutral or slightly alkaline. The reaction was completed after 30 minutes. The mixture was slightly acidified with hydrochloric acid, diluted with water and extracted with ether. The ether extract was dried and concentrated in vacuo. Upon the addition of ether to the oily residue, the product, 2-chloroacetamido-5-chlorobenzophenone (3-oxime, crystallized in colorless prisms melting at 161°-162°C. 

Inorganic compound extraction, ionic liquids in, 26 875-876 Inorganic compound-hydrogen chloride-water systems, 13 817-818 Inorganic compound lubricants, 15 246 Inorganic compounds, 13 104 hydrochloric acid reaction with,... 

Add tin dichloride and sulphurous acid solutions respectively to two test tubes containing solutions of tellurium(IV) oxide in hydrochloric acid diluted with water. Heat the contents of the test tubes. Comment on your observatioss. WriteJjie equations of the reactions. What property do the salts of tetravalent tellurium exhibit in the given reactions ... 

Add 8.0g (10.0ml, 0.15 mol) of redistilled acrylonitrile (Expt 5.161, Note (1)) to a stirred solution of diethyl propylmalonate (30.2 g, 0.15 mol) (Expt 5.132) and of 30 per cent methanolic potassium hydroxide (4.0 g) in t-butyl alcohol (100 g). Keep the reaction mixture at 30-35 °C during the addition and stir for a further 3 hours. Neutralise the solution with 2 M-hydrochloric acid, dilute with water and extract with ether. Dry the ethereal extract with anhydrous sojdium sulphate and distil off the ether the residue [diethyl (2-cyanoethyl)-propylmalonate 11 g] solidifies on cooling in ice, and melts at 31—32 °C after recrystallisation from ice-cold ethanol. Boil the cyanoethyl ester (10 g) under reflux with 40 ml of 48 per cent hydrobromic acid solution for 8 hours, and evaporate the solution almost to dryness under reduced pressure. Add sufficient water to dissolve the ammonium bromide, extract several times with ether, dry the ethereal extract and distil off the solvent. The residual oil (4.5 g, 66%) soon solidifies upon recrystallisation from water, pure 2-propylglutaric acid, m.p. 70 °C, is obtained. 

Bromo-4-chlorobutanoyl bromide (300 mmol) was added to a solution of N-methylaniline (320 mmol) and triethylamine (330 mmol) in toluene (340 mL). The reaction was exothermic, and the mixture was cooled to maintain the temperature at about 40°C. After the addition was complete, the resulting mixture was stirred for 30 minutes, 150 mL water was added, and the mixture was stirred further. The aqueous and organic phases were separated, and the organic phase was washed with 5% hydrochloric acid and with water. The toluene was evaporated completely under vacuum to yield 86.3 g 2-bromo-4-chloro-N-methyl-N-phenylbutanamide (98% yield, approximately 95-96% pure). 

To a stirred solution of methyl magnesium iodide (748 mg, 4.5 mmol) in ether (15 ml), diphenyliodonium bromide (722 mg, 2 mmol) and anhydrous nickel chloride (15 mg) were added all at once at room temperature, under nitrogen. The mixture was stirred for 20 min, unreacted methyl magnesium iodide was decomposed by addition of water, the reaction mixture was neutralized with 10% hydrochloric acid, washed with water, and the ether layer dried and concentrated. The residue was chromatographed (silica, petroleum ether) to give the pure biaryls. 

Aminoazo dyes with only one amino group (aminoazobenzene type) are weak bases giving, in general, difficultly soluble salts which are readily hydrolyzed. If the dye is to be isolated as one of its salts, for example, the hydrochloride, the salt is precipitated from the reactiorr mixture by means of a considerable excess of hydrochloric acid. The precipitate is filtered off and washed with dilute hydrochloric acid, not with water. On the other hand, if the dye is to be used in coloring oils, fats, etc., it must be isolated as the free base and must contain no salts. For this purpose, the coupling reaction mixture is made alkaline and the precipitated dye is filtered off and washed thoroughly with water. The dye can be purified further by.recrystallization from an organic solvent. 

B. 1,2-Bis n-butylthio)benzem. In a 1-1., round-bottomed, three-necked flask fitted with a reflux condenser, a mechanical stirrer, and a thermometer which reaches into the reaction mixture is placed a solution of 59.0 g. (0.25 mole) of o-dibromobenzene in a mixture of 250 ml. of quinoline and 80 ml. of pyridine. To this solution is added 84.0 g. (0.55 mole) of cuprous -butylmer-captide, and the mixture is stirred and heated under reflux (Note 5) for 3.5 hours (Note 6). Heating is stopped and the reaction mixture is allowed to cool to about 100°. It is then poured into a stirred mixture of 1500 g. of ice and 400 ml. of concentrated hydrochloric acid occasional stirring is continued for about 2 hours. The aqueous part is then decanted from the dark brown, gummy residue and is extracted twice with 400 ml. portions of ether. The ether extract is added to the residue, and the resulting mixture is stirred for about 5 minutes. The ether solution is then decanted from the residue and is filtered. The residue is extracted twice more with 400-ml. portions of ether (Note 7). The combined ether extract is washed twice with 100-ml. portions of 10% hydrochloric acid, once with water, and twice with 100-ml. portions of concentrated ammonia (Note 8). After a final wash with water, the ether solution is dried over anhydrous potassium carbonate. The potassium carbonate is collected on a filter, and the ether is removed from the filtrate by distillation. The remaining brown oil is distilled in vacuum, giving a pale orange oil, b.p. 123-124°/0.3 mm., d 1.5684. The yield is 46.5-56.0 g. (73-87%) (Note 9). 

I) Isocyanide Reaction of Primary Amines. Place 1 drop of aniline in one test tube, and 1 drop of n butylamine in another. Add to each 3 or 4 drops of chloroform and 1 ml of alcoholic potash. Use the hood.) Warm it for a few seconds. The isocyanides can be recognized by the odor. Clean the tube with concentrated hydrochloric acid, then with water. Write the equation for the reaction. What is the structure of isocyanide ... 

EXPLOSION and FIRE CONCERNS flammable liquid when exposed to heat, flame, or oxidants NFPA rating Health 2, Flammability 2, Reactivity 0 dangerous explosion hazard reacts vigorously with oleum and chlorosulfonic acid reaction with water or steam produces toxic and corrosive fumes formation of peroxides may occur in containers that have been opened and remain in storage incompatible with strong oxidizers decomposes in the presence of moisture to form hydrochloric acid use dry ehemical, foam, carbon dioxide, or water spray for firefighting purposes. 

SULPHANILAMIDE. (Reaction C.) Add 15 g. of the above thoroughly drained sulphonamide to 10 ml. of concentrated hydrochloric acid diluted with 20 ml. water, and boil the mixture gently under reflux for i hour. Then add 30 ml. of water and heat the mixture again to boiling, with the addition of a small quantity of animal charcoal. Filter the boiling solution, and add powdered sodium carbonate in small quantities to the filtrate with stirring until all eflFervescence ceases and the sulphanilamide is precipitated as a white powder. Cool the mixture thoroughly and filter oflF the sulphanilamide at the pump, wash with water and dry. Yield, ca. 10 g. 

Finally, add an excess of concentrated hydrochloric acid slowly with stirring to the alkaline filtrate remaining from the original reaction product. As the solution becomes acid, the sulphonyl-aniline separates as a thick sticky syrup which, when stirred, rapidly crystallises. Cool the mixture in ice-water if necessary, and then filter off the solid product at the pump, wash well with water, and drain. Recrystallise from a mixture of 2 volumes of ethanol and i volume of water to prevent the sulphonyl-aniline from separating as an emulsion, allow the hot solution to cool spontaneously (with occasional stirring) until crystallisation starts, and... 

The determination of tin in metals containing over 75 wt % tin (eg, ingot tin) requites a special procedure (17). A 5-g sample is dissolved in hydrochloric acid, reduced with nickel, and cooled in CO2. A calculated weight of pure potassium iodate (dried at 100°C) and an excess of potassium iodide (1 3) are dissolved in water and added to the reduced solution to oxidize 96—98 wt % of the stannous chloride present. The reaction is completed by titration with 0.1 Af KIO —KI solution to a blue color using starch as the indicator. 

At 180°C, reaction with water results in formic acid, methyl chloride, methanol, hydrochloric acid, and some carbon monoxide. 

To produce a moulding composition, aniline is first treated with hydrochloric acid to produce water-soluble aniline hydrochloride. The aniline hydrochloride solution is then run into a large wooden vat and formaldehyde solution is run in at a slow but uniform rate, the whole mix being subject to continuous agitation. Reaction occurs immediately to give a deep orange-red product. The resin is still a water-soluble material and so it is fed into a 10% caustic soda solution to react with the hydrochloride, thus releasing the resin as a creamy yellow slurry. The slurry is washed with a counter-current of fresh water, dried and ball-milled. 

Copiously flush eyes with water for up to 15 min, and skin with water and soap - except in the case of substances such as quicklime whose reaction with water is exothermic (1 g generates >18 kcal), titanium or tin tetrachloride, both of which rapidly hydrolize to form hydrochloric acid... 

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