Sodium carbonate reaction with hydrochloric acid

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. 

One method of preparing sulphlnic acids has already been described (diazo reaction. Section IV,65). Reduction of a sulphonyl chloride with zinc powder and water affords the zinc salt of the sulphinic acid, converted by sodium carbonate to the sodium salt (in which form it is conveniently isolated), and by hydrochloric acid into the somewhat unstable sulphinic acid, for example ... 

A mixture of 1.0 g of 6,6,9-trimethyl-9-azabicyclo[3.3.1 ] nonan-3/3-ol, methyl 0i,0i-di-(2-thienyD-glycollate and 30 mg of metallic sodium is heated at 80°C to 90°C for about 2 hours under reduced pressure. After cooling, ether is added to the reaction mixture. The mixture is extracted with 10% hydrochloric acid. The aqueous layer is alkalified with sodium carbonate and reextracted with ethyl acetate. The extract is washed with water, dried and concentrated to dryness. The residue thus obtained is treated with hydrogen chloride by conventional manner. 2.0 g of the 0i,0i-di-(2-thienyl)glycollate of 6,6,9-trimethyl-9-azabicyclo-(3.3.1 ] nonan-3/3-ol hydrochloride are obtained. Yield 83%. 

The mixture is cooled and poured onto a mixture of 200 ml. of 6N hydrochloric acid, 200 ml. of ether, and 100 g. of ice. The residue in the flask is dissolved in a mixture of 6N hydrochloric add and methylene chloride, and this mixture is added to the main reaction. The aqueous layer is separated and extracted with two lOO-ml. portions of ether. The combined ethereal solution is washed once with 70 ml. of 6N hydrochloric acid, once with 2N sodium carbonate solution, twice with saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure, and the residue is distilled to >ield 16-17 g. (72-76%) of colorless 2-benzylcyclo-pentanone, b.p. 83-85° (0.3 mm.), 108-110° (0.75 nun.) (Note 13). 

Sodium carbonate was made historically by the Leblanc process. The first commercial production was carried out by the Leblanc process. In this process, sodium chloride was treated with sulfuric acid to produce sodium sulfate and hydrochloric acid. Heating the sodium sulfate with coal and limestone produced a black ash that contained sodium carbonate, calcium sulfide, unreacted coal, and calcium carbonate. Sodium carbonate was separated from the black ash by leaching with water. The overall reaction is as follows ... 

To a stirred solution of 120 ml of methylene chloride, 18 ml of dry pyridine, and 5 ml of iodine pentafluoride maintained at —10°C to —20°C in a Dry Ice-carbon tetrachloride slurry is added a solution of 13.5 gm (0.1 mole) of cumyl-amine in 10 ml of methylene chloride over a 1 hr period. The reaction mixture is stirred for another hour at —10°C, and then for 1 hr at 0°. After this time, water is added to the reaction mixture and stirring is continued until the yellow solid which had formed is dissolved. The lower organic layer is separated and washed in turn with water, 1 N hydrochloric acid, a saturated sodium thiosulfate solution, and again with water. After drying with anhydrous magnesium sulfate and filtration, the product solution is partially evaporated by means of a rotary evaporator at a temperature below 30°C. The brown solid obtained on cooling is separated and recrystallized twice from methylene chloride yield 4.75 gm (17.9%), m.p. 86.9°-88.7°C. 

Samples of the niobium (V) chloride or niobium (V) bromide-pyridine reaction mixtures were hydrolyzed in concentrated hydrochloric acid. Aliquots were diluted and neutralized with sodium carbonate to a pH of approximately 8. Sodium tetraphenylborate(III) solution then was added and a precipitate of l-(4-pyridyl) pyridinium tetraphenylborate(III) was produced. The precipitate was filtered and extracted with concentrated hydrochloric acid. The ultraviolet absorption spectrum of the extract is shown in Figure 3 for comparison with the spectrum of a known sample of l-(4-pyridyl) pyridinium dichloride in dilute hydrochloric acid. 

Neither hydrochloric nor nitric acid initiates a self-sustained reaction in powder stabilized with sodium carbonate or magnesium oxide. 

Ogner [1] has described an automated analyser method for the determination of boron-containing anions in plants. This is based on the formation of a fluorescent complex between these anions and carminic acid at pH 7. The plant tissues are ashed at 550 °C and the residue dissolved in 0.5 N hydrochloric acid prior to adjustment to pH 6-7 with sodium carbonate solution. The solution is excited at 470 nm and fluorescence intensities measured at 585 nm. Interferences by the reaction of some cations with carminic acid are overcome by passing the solution through an ion exchange column to exchange the cations for sodium ions. Analytical recoveries of boron anions were in the range 98-104%. The detection limit of the method was 5 xg/l boron. 

Wear nitrile rubber gloves, laboratory coat, and eye protection. Cover spill with a 1 1 1 mixture by weight of sodium carbonate or calcium carbonate, clay cat litter (bentonite), and sand. Scoop into a container and remove to fume hood. Slowly add the solid mixture to a large volume of stirred water and crushed ice in a beaker. When the reaction is complete, neutralize with sodium carbonate or dilute hydrochloric acid. Decant the liquid... 

A mixture of 100 kg of 8-benzyltheophilline, 36 L of N-ethylethanolamine, 300 L of 1,2-dichlorethane and 71 kg of sodium carbonate was refluxed for 24 hours. Then 36 L of N-ethylethanolamine was added and the reaction mixture was refluxed. After cooling to the mixture was added the water and hydrochloric acid. The organic phase was extracted with hydrochloric acid. The acidic phase was neutralized with sodium carbonate and the 7-(N-ethyl-N-p-hydroxyethylaminoethyl)-8-benzyltheophilline was extracted with dichloromethane. The solvent was evaporated and the free base of 7-(N-ethyl-N-p-hydroxyethylaminoethyl)-8-benzyltheophilline was dissolved in methanol. Hydrochloride of 7-(N-ethyl-N-p-hydroxyethylaminoethyl)-8-benzyltheophilline was obtained by addition to the solution the hydrochloric acid yield 81%, melting point 185-186°C. 

About 55.5 g of p-chloroethyl-di-n-butylcarbamate and about 22.6 g of dimethylamine are placed in a container, firmly sealed, and heated at about 95°C for about 16 hours. To the resulting crude mixture is added ethyl ether and the mixture filtered to remove dimethylamine hydrochloride formed during the course of the reaction. The ethereal solution is then extracted with 12 N hydrochloric acid. Under a fresh layer of ether and at a temperature under 10°C the aqueous acid extract is first neutralized with sodium carbonate and then made strongly alkaline with sodium hydroxide. The supernatant ethereal solution is then separated and dried over potassium hydroxide. The ethereal solution is finally concentrated and the residue obtained is fractionally distilled under vacuum. The p-dimethylaminoethyl-di-n-butylcarbamate is found to distill undecomposed at about 128°C to 130°C under approximately 2 mm pressure. 

A mixture of potassium hydroxide in methanol (300 ml) and water (5 mL) is added to [3aR-[3aa,4a(lE,3S),5p,6aa]]-5-(benzoyloxy)hexahydro-4-(3 -hydroxy-5-phenyl-l-pentyl)-2H-cyclopenta[b]furan-2-one. The mixture is stirred and heated in an 80°C for 2 hours. When the reaction is complete, the mixture is concentrated under reduced pressure. Water (100 mL) and MTBE (100 mL) are added and the mixture stirred at 20-25°C for 15 min. The phases are allowed to separate. The product is in the aqueous phase and the organic phase is removed. The pH of the aqueous phase is adjusted to 1 to 1.5 by the addition of hydrochloric acid (3 N, about 60 mL are required). The solution is stirred at 20-25°C. After 30 min, MTBE (100 mL) is added and the mixture stirred for 12 hours. The phases are separated and the aqueous phase extracted once with MTBE (50 mL). The MTBE phases are combined and washed with sodium carbonate (1 N, 50 mL). The MTBE mixture is stirred with a solution of potassium hydroxide (2.8 g, 42.5 mmole) in water (100 mL) for 30 min. The phases are separated and the aqueous phase is added to a slurry... 

The test is usually carried out by adding the reagent to the solution acidified with dilute hydrochloric acid carbonates, sulphites, and phosphates are not precipitated under these conditions. Concentrated hydrochloric acid or concentrated nitric acid should not be used, as a precipitate of barium chloride or of barium nitrate may form these dissolve, however, upon dilution with water. The barium sulphate precipitate may be filtered from the hot solution and fused on charcoal with sodium carbonate, when sodium sulphide will be formed. The latter may be extracted with water, and the extract filtered into a freshly prepared solution of sodium nitroprusside, when a transient, purple colouration is obtained (see under Sulphides, Section IV.6, reaction 5). An alternative method is to add a few drops of very dilute hydrochloric acid to the fused mass, and to cover the latter with lead acetate paper a black stain of lead sulphide is produced on the paper. The so-called Hepar reaction, which is less sensitive than the above two tests, consists of placing the fusion product on a silver coin and moistening with a little water a brownish-black stain of silver sulphide results. 

Cleaning Up Add the water from the gas trap to the combined aqueous filtrates from all reactions and neutralize the solution by adding either 10% hydrochloric acid or sodium carbonate. Flush the neutral solution down the drain with a large excess of water. Any spilled drops of chlorosulfonic acid should be covered with sodium carbonate, the powder collected in a beaker, dissolved in water, and flushed down the drain. 

Cleaning Up The aqueous layer from the first part of the reaction should be neutralized with sodium carbonate, diluted with water, and flushed down the drain. The aqueous layer containing hydrosulfite, saturated sodium chloride, and sodium hydroxide are treated with household bleach (5.25% sodium hypochlorite solution) until no further reaction is evident. After neutralizing the solution with dilute hydrochloric acid, the solution is diluted with water and flushed down the drain. Shake the mixture of silver oxide, silver, and sodium sulfate with water to dissolve the sodium sulfate, and then recover the mixture of silver and silver oxide by vacuum filtration. 

Procedure for the Determination of the Percent Yield of Sodium Chloride Formed by Reaction of Sodium Carbonate with Hydrochloric Acid... 

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