Sodium acetate, anhydrous fused

Dissolve 1 0 g. (or 10 ml.) of the amine and 1 0 g. of 2 4-dinitrochloro-benzene in 5-10 ml. of ethanol, add a slight excess of anhydrous potassium carbonate or of powdered fused sodium acetate, reflux the mixture on a water bath for 20-30 minutes, and then pour into water. Wash the precipitated solid with dilute sodium carbonate solution, followed by dilute hydrochloric acid. Recrystallise from ethanol, dilute alcohol or glacial acetic acid. 

Commercial acetic acid is manufactured fiom pyroligneous acid obtained in the destructive distillation of wood. The latter is neutralised with lime, and separated by distillation from wood-spirit and acetone. The crude calcium acetate, which has a dark colour, is then distilled with the requisite quantity of concentrated hydrochloric acid. Anhydrous or glacial acetic acid is obtained by distilling fused sodium acetate with concentrated sulphuric acid. 

Bismuth(III) acetate catalyzes the synthesis of azlactones (17) from aromatic aldehydes in moderate to good yields via the Erlenmeyer synthesis. While the standard procedure for azlactone synthesis consists of using a stoichiometric amount of fused anhydrous sodium acetate, 10 mol% of Bi(OAc)3 is sufficient to catalyze the reaction and the crude product is found to be > 98% pure. 

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. 

Phenyl cinnamate and other phenolic esters have been prepared by heating the acid and phenol in the presence of phosphorus oxychloride,1 and by heating the acid anhydride and phenol together in the presence of a dehydrating agent such as fused zinc chloride or anhydrous sodium acetate.2 Phenyl cinnamate has also been prepared by the careful distillation of phenyl fumarate.3... 

When sodium chloride is fused with anhydrous chromium(II) chloride the product is NaCrCI5 regardless of the proportions of chlorides used.222 Other cations give tetra- or tri-chloro-chromates(II) as in Sections 35.3.7.3.ii and 35.3.7.3.vi above. The solvate [pyH]3[CrBr5]-2MeC02H has been isolated from the metal acetate and pyridine in a mixture of acetyl bromide and acetic acid, and there is considerable splitting of the spin-allowed d-d band in the reflectance spectrum of this complex,255 but no detailed investigations of pentahalochromates have been reported. 

Esterification is effected in the cold in presence of alkali or by heating the alcohol and anhydride together, usually in presence of a dehydrating agent—e.g., fused zinc chloride, anhydrous sodium acetate, etc. Preparation 204.—Mannitol Hexacetate. 

Dihydro-1,2,4-benzotriazine-3-thiones (171a,b) react with halo-genoacid in the presence of fused sodium acetate in anhydrous ethanol to... 

Sodium acetate (trihydrate), (M.Wt. 136.08). Cryst. from aq. ethanol.(The anhydrous salt can be prepared by heating the trihydrate slowly till it hquefies, steam is evolved and the mass again solidifies. Heating is increased slowly, to avoid charring, until the salt again fuses. After several minutes it is allowed to cool, is powdered and bottled.)... 

Mix 10 ml of the oil, 20 ml of acetic anhydride (95 to 100 per cent), and 2 g of freshly fused anhydrous sodium acetate in a long-necked, round-bottomed, 200-ml Kjeldahl flask add a fragment of broken glass and boil the contents gently under an air reflux condenser for two hours. Support the flask on a sheet of asbestos board, in which has been cut a hole about 11 inches in diameter, and heat by a small naked flame, placed about 1 inch below% and not impinging on the bottom of the flask. 

Reagents acetic anhydride, freshly fused sodium acetate, sodium carbonate, anhydrous pyridine. 

The characteristic colours and solubilities of many metallic sulphides have already been discussed in connection with the reactions of the cations in Chapter III. The sulphides of iron, manganese, zinc, and the alkali metals are decomposed by dilute hydrochloric acid with the evolution of hydrogen sulphide those of lead, cadmium, nickel, cobalt, antimony, and tin(IV) require concentrated hydrochloric acid for decomposition others, such as mercury(II) sulphide, are insoluble in concentrated hydrochloric acid, but dissolve in aqua regia with the separation of sulphur. The presence of sulphide in insoluble sulphides may be detected by reduction with nascent hydrogen (derived from zinc or tin and hydrochloric acid) to the metal and hydrogen sulphide, the latter being identified with lead acetate paper (see reaction 1 below). An alternative method is to fuse the sulphide with anhydrous sodium carbonate, extract the mass with water, and to treat the filtered solution with freshly prepared sodium nitroprusside solution, when a purple colour will be obtained the sodium carbonate solution may also be treated with lead nitrate solution when black lead sulphide is precipitated. 

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