Sodium, acetate, evaporation

Ash is a measure of residual sodium acetate. A simple method consists of dissolving the PVA in water, diluting to a known concentration of about 0.5 wt %, and measuring the electrical conductivity of the solution at 30°C. The amount of sodium acetate is estabUshed by comparing the result to a cahbration curve. A more lengthy method involves the extraction of the PVA with methanol using a Soxhlet extractor. The methanol is evaporated and water is added. The solution is titrated using hydrochloric acid in order to determine the amount of sodium acetate. 

A solution of 16jS-methyl-l la,17a,21-trihydroxy-5j5-pregnane-3,20-dione 21-acetate (52), 45 g, in dioxane (297 ml) is cooled to 15° and treated over a 5 min period with a solution of bromine (34.2 g) in dioxane (594 ml) precooled to 18°. After 2 min a solution of sodium acetate (60 g) in water (600 ml) is added and the mixture poured into ice water (8 liters). The precipitate is filtered off, washed to neutrality with water, and dried to give the crude dibromide (53), 55.7 g mp 125-126° (dec.) [aJu 58°. A mixture of dibromide (53), 55.5 g, lithium bromide (27.8 g), lithium carbonate (27.8 g) and DMF (1.11 liters) is refluxed under rapid stirring for 6 hr. The mixture is concentrated under vacuum to about 250 ml, poured into ice water (8 liters) containing hydrochloric acid (250 ml), and extracted with methylene dichloride. The extracts are washed to neutrality with water and evaporated to dryness. The residue is dissolved in acetone, evaporated to dryness under reduced pressure, redissolved in acetone and crystallized by the additon of hexane. This gives the dienone (54) 24.4 g, mp 236-239°. 

The residue (12 g) which contains the 18-iodo-18,20-ether is dissolved in 200 ml of acetone, 5 g of silver chromate is added Note 3) and after cooling to 0°, 11.8 ml of a solution of 13.3 g of chromium trioxide and 11.5 ml of concentrated sulfuric acid, diluted to 50 ml with water is added during a period of 5 min. After an additional 60 min, a solution of 112 g of sodium acetate in 200 ml of water is added and the mixture diluted with benzene (400 ml), filtered and the benzene layer separated. The aqueous phase is reextracted with benzene, washed with half-saturated sodium chloride solution, dried and evaporated to yield 11.2 g of a crystalline residue. Recrystallization from ether gives 7.2 g (72%) of pure 3/5, 1 la, 20/5-trihydroxy-5a-pregnan-18-oic acid 18,20 lactone 3,11-diacetate mp 216-218°. 

The crude residue is dissolved in about 10 ml of acetone and treated at 0° with 0.6 ml 8 N chromic acid in sulfuric acid. After 45 min at 0°, 6 g sodium acetate in 10 ml water and 20 ml of benzene are added and the organic phase is separated, dried and evaporated under reduced pressure whereby 0.61 g of crude product is obtained. 

Solid sodium nitrite (0.97 g) was added at room temperature with stirring over a period of one hour to a solution of 2-chloro-9-(2-hydroxyethoxymethyl)adenine (0.5 g) in glacial acetic acid (10 ml). The reaction mixture was stirred for an additional A A hours. The white solid was removed by filtration, washed with cold acetic acid and then well triturated with cold water to remove the sodium acetate present. The solid product was retained. The combined acetic acid filtrate and wash was evaporated at reduced pressure and 40°C bath temperature and the residual oil triturated with cold water. The resulting solid material was combined with the previously isolated solid and the combined solids dried and recrystallized from ethanol to give 2chloro-9-(2-hydroxyethoxymethyl)+iypoxanthine (0.25 g), MP>310°C. Elemental analysis and NMR spectrum were consistent with this structure. 

The solvent was evaporated off under reduced pressure, and the residual gum refluxed with concentrated hydrochloric acid (50 g) for 6 hours. The solution was aliowed to cool overnight. It was filtered from the phthalic acid crystals, and freeze-dried, and to the pink residue was added acetone (160 g) and ethyl acetate (50 g). The mixture was left in the cold room overnight and the clear pink supernatant liquid poured off. The pink gummy hydrochloride remaining in the flask was dissolved in water (20 g), saturated sodium acetate solution added until precipitation was complete, and the product collected and dried in a desiccator. The crude p-bis-(2-chloroethyl)-aminophenylalanine (3.6 g) was crystallized from methanol giving colorless needles, MP 172° to 174°C (decomp.) of p-bis-(2-chloroethyl)-aminophenylalanine. 

The resulting mixture does not crystalize and is converted into a mixture of oximes by treatment of a solution of the mixture in 20 ml of ethanol with a solution of 1.8 g of hydroxylamine sulfate in 3 ml of water. 1.B g of sodium acetate In 5 ml of water is added, and the mixture is refluxed for 5 hours, then extracted with ethyl acetate, and the ethyl acetate solution is washed with a saturated aqueous sodium chloride solution and dried over Sodium sulfate. After evaporating the solvent, the residue is triturated with warm ether and 1.1 g of a crystalline oxime is obtained, MP 16B° to 171°C. 

Evaporation gives the salt sodium acetate, which contains Na+ and CH3COO ions. Many of the salts of carboxylic acids have important uses. Sodium and calcium propionate (Na+ or Ca2+ ions, CH3CH2COO ions) are added to bread, cake, and cheese to inhibit the growth of mold. 

Procedure. The test solution should contain between 0.001 and 0.02 mg of cobalt. Evaporate almost to dryness, add 1 mL of concentrated nitric acid, and continue the evaporation just to dryness to oxidise any iron(II) which may be present. Dissolve the residue in 10 mL of water containing 0.5 mL each of 1 1 hydrochloric acid and 1 10 nitric acid. Boil for a few minutes to dissolve any solid material. Add 2.0 mL of a 0.2 per cent aqueous solution of nitroso-R-salt and also 2.0 g of hydrated sodium acetate. The pH of the solution should be close to 5.5 check with bromocresol green indicator or with a pH meter. Boil for 1 minute, add 1.0 mL of concentrated hydrochloric acid, and boil again for... 

A mixture of 2.65 g. of freshly distilled 2,3-O-isopropylidene-D-glycerose, 1.5 ml. of ethyl acetoacetate, 0.7 g. of zinc chloride, 20 ml. of N sulfuric acid, and 20 ml. of 96% ethyl alcohol is kept at room temperature for twenty-four hours. After addition of 3 g. of crystalline sodium acetate and keeping for a further 48 hours at room temperature, the mixture is heated for 15 minutes at 90°. It is then repeatedly extracted with ether, and the united extracts are successively washed with water, an aqueous solution of sodium bisulfite, and a small quantity of aqueous sodium hydroxide solution. The ether layer is dried with anhydrous sodium sulfate and the solvent is evaporated, yielding an oil which is saponified with aqueous sodium hydroxide solution (4 ml. of 10%) by heating on a steam bath for one hour. The aqueous solution is extracted with ether, acidified (to Congo Red) with phosphoric acid, and then repeatedly extracted with ether the united extracts are dried with anhydrous sodium sulfate and the solvent is evaporated, giving a residue which crystallizes from water yield, 0.2 g. of the product (X) m. p., 153-155°. 

Triphenylmethyl sodium and triphenylmethyl potassium conduct in liquid ammonia although they slowly react with that solvent.887 888 When the liquid ammonia is allowed to evaporate from a solution of triphenylmethyl sodium in ammonia, the residue is a colorless mixture of sodamide and triphenylmethane. The sodium-tin and sodium-germanium compounds analogous to sodium triphenylmethide are also strong electrolytes in liquid ammonia. Sodium acetylide in liquid ammonia is dissociated to about the same extent as sodium acetate in water.889... 

What is the evaporation rate and yield of the sodium acetate hydrate CH3C00Na.3H20 from a continuous evaporative crystalliser operating at 1 kN/m2 when it is fed with 1 kg/s of a 50 per cent by mass aqueous solution of sodium acetate hydrate at 350 K The boiling point elevation of the solution is 10 degK and the heat of crystallisation is 150 kJ/kg. The mean heat capacity of the solution is 3.5 kJ/kg K and, at 1 kN/m2, water boils at 280 K at which temperature the latent heat of vaporisation is 2.482 MJ/kg. Over the range 270-305 K, the solubility of sodium acetate hydrate in water s at T(K) is given approximately by ... 

To 136 g A4 carene in 330 ml methylene chloride and 120 g anhydrous sodium acetate, add dropwise with vigorous stirring ir an ice bath, 167 g of 50% peracetic acid and continue stirring for ten hours. Heat to boiling for two hours, cool, wash with water, sodium carbonate, water, and dry, evaporate in vacuum the methylene chloride to get about 100 g p-menthadieneol. Apparently (CA... 

A (Alternative) JCS 3175(1952). 2 g 3-indolyl-acetic acid (preparation given elsewhere here), 1.55 g freshly fused sodium acetate, 5 ml acetic anhydride. Heat 135-140° on oil bath for eighteen hours cool, wash with water and extract with CHCl3-ether (1 4). Wash organic phase with 3X20 ml saturated KHC03 and dry, evaporate in vacuum to get the l-acetyl-3-indolyl-acetone, which can be reduced to the alpha-methyl-tryptophol derivative with lithium aluminum hydride, and then converted to the dialkyl-tryptamine as already described (as can (I)), or used in step B, or reduced to (I) as follows dissolve 1 g in 1 ml 1 N Na-methoxide in methanol and 60 ml methanol, and keep at 40° for 10 minutes acidify with dilute HC1 and extract with ether. Dry, evaporate in vacuum to get (I) (recrystallize-methanol). 

A mixture of 9.5 g pyrrolyl-2-aldehyde, 29.2 g dimethyl-succinate and NaH (9.6 g of 50% suspension in oil) in 100 ml benzene is stirred at room temperature 6 hours, cooled and carefully acidified with glacial acetic acid. Add water and ether and dry, evaporate in vacuum or work up (JACS 72,501 (1950), JCS 1025(1959)) to get ca. 17 g (80%) 3-methoxycarbonyl-4-(2 -pyrrolyl)-3-butenoic acid (I) (recrystallize-acetone-benzene). A mixture of 12 g (I), 7 g sodium acetate and 70 ml acetic anhydride is left overnight at room temperature with occasional shaking. Then gradually raise the temperature to 70-75° over 2 hours, maintain for 4 hours and work up (see JCS 1714(1955), 986( 1958)) to get ca. 8 g (60%) methyl-4-acetoxy-indole-6-carboxylate (II) (recrystallize-petroleum ether). If desired, this can be converted to 4-OH-indole-6-COOH and 4-methoxyindole-COOH as described in the ref. or decarboxylated as described elsewhere here. If the 1-methyl cpd. is used, 1-Me-indole results. 

Add 0.44 moles ring substituted phenylacetate, 100 g acetic anhydride and 30 g sodium acetate and heat at 145-150° for 18 hours to get ca. 0.4 moles of the methyl-phenylacetate (I). Add (I) and formamide (or N-methyl-formamide for the N-methyl cpd.), heat 4-5 hours at 180-195°, cool and extract with CHC13. Evaporate in vacuum, dissolve residue in 40% sulfuric acid and heat at 90-125° for 5-6 hours. Neutralize and add solid NaOH to precipitate about 50% amphetamine. Treat with 10% sulfuric acid to get the sulfate. 

Preparation of Anhydrous Sodium Acetate.—The hydrated salt (3 H20) is heated over a naked flame in a shallow iron or nickel dish. After the water of crystallisation has evaporated the material solidifies. By careful heating the anhydrous salt is now also fused. After resolidification the still warm substance is powdered and immediately transferred to an air-tight container. Commercial anhydrous acetate should also be fused before use. 

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