Crystal ammonia

A. Gas-Solid Reactions in Polar Crystals Ammonia-p-Bromobenzoic... 

Hydrates and ammoniates.—Judging from records of salts with water of crystallization and also with ammonia of crystallization, ammonia, in its tendency to unite with other compounds, probably exceeds water. Just as a salt may unite with water to form a hydrate, so can salts combine with ammonia to form ammoniates, or ammines, e.g. oupric and mercurio chlorides form respectively Cuda.2NH3 and HgCl2.2NH3, etc. 

Synonyms CAS 506-87-6 carbonic acid, ammonium salt diammonium carbonate CRYSTAL AMMONIA AMMONIUM SESQUICARBONATE HARTSHORN... 

In the commercial extraction of alkaloids from the drugs in which they exist, the powdered drug, or an alcoholic extract of it, is treated with an alkali such as ammonia or lime to liberate the alkaloid and the alkaloid is then extracted by means of an organic solvent. The crude material thus obtained is purified and finally crystallized either as the base itself or as its water-soluble salts. 

Colourless crystals m.p. 50 C, b.p. 301 C. Basic and forms sparingly soluble salts with mineral acids. Prepared by the reduction of 1-nitronaphthalene with iron and a trace of hydrochloric acid or by the action of ammonia upon l-naphlhol at a high temperature and pressure. 

The hexahydrate fonns colourless crystals, m.p. 44 C (104 C when anhydrous), b.p. 126 C. Made by the action of alcoholic ammonia on 1,2-dichloroethane, piperazine is used in human and veterinary medicine in the treatment of threadworm and roundworm infestations. 

QHgNiOiS. Colourless crystals, m.p. 164 5-166-5" C. It is usually prepared by treating p-acetamidobenzenesulphonyl chloride with ammonia, and hydrolysing the acetyl derivative to the base. Used for the treatment of streptococcal infections, gonorrhoea, meningococcal meningitis and urinary infections. Liable to cause unpleasant reactions, such as nausea, cyanosis and skin rashes. 

The addition of potassium to Fe single crystals also enliances the activity for ammonia synthesis. Figure A3.10.19 shows the effect of surface potassium concentration on the N2 sticking coefficient. There is nearly a 300-fold increase in the sticking coefficient as the potassium concentration reaches -1.5 x 10 K atoms cm ... 

Bare S R, Strongin D R and Somoqai G A 1986 Ammonia synthesis over iron single crystal catalysts—the effects of alumina and potassium J. Phys. Chem. 90 4726... 

Succinamide. NHoCOCH2 CH2CONH2. (Method 2(a)). Add 5 ml. (5 8 g.) of dimethyl succinate to a mixture of 50 ml. of water and 25 ml. of concentrated [dy o-88o) aqueous ammonia solution in a 150 ml. conical flask. Cork the flask and shake the contents the dimethyl succinate rapidly dissolves to give a clear solution. Allow the solution to stand after about i hour the succinamide starts to crystallise, and then continues to separate for some time. Next day, filter off the succinamide at the pump, wash with cold water, and drain. Recrystallise from water, from which the succinamide separates as colourless crystals the latter soften at 240° and melt at 254 -255° with... 

Place I g. of benzamide and 15 ml. of 10% aqueous sodium hydroxide solution in a 100 ml. conical flask fitted with a reflux water-condenser, and boil the mixture gently for 30 minutes, during which period ammonia is freely evolved. Now cool the solution in ice-water, and add concentrated hydrochloric acid until the mixture is strongly acid. Benzoic acid immediately separates. Allow the mixture to stand in the ice-water for a few minutes, and then filter off the benzoic add at the pump, wash with cold water, and drain. Recrystallise from hot water. The benzoic acid is obtained as colourless crystals, m.p. 121°, almost insoluble in cold water yield, o 8 g. (almost theoretical). Confirm the identity of the benzoic acid by the tests given on p. 347. 

To prepare the hydrochloride, add about i g. of aminoazobenzene to 200 ml. of dilute hydrochloric acid and boil until nearly all the solid material has dissolved. Filter hot and allow to cool slowly. Aminoazobenzene hydrochloride separates as beautiful steel-blue crystals filter and dry. If a small quantity of the powdered hydrochloride is moistened with water and a few drops of ammonia added, the blue hydrochloride is converted back to the yellowish-brown base. 

Place 5 ml. of benzaldehyde in a wide-necked stout-walled bottle of about 100 ml. capacity (a conical flask is too fragile for this purpose) and add 50 ml. of concentrated dy 0 880) ammonia solution. Cork the bottle securely, shake vigorously, and then allow to stand for 24 hours, by which time the layer of benzaldehyde at the bottom of the bottle will have been converted into a hard mass of hydrobenzamide. (If after 24 hours the crude hydrobenzamide is still syrupy, shake the mixture vigorously and allow to stand for another hour, when the conversion will be complete.) Break up the solid pellet with a strong spatula, filter at the pump, wash with water and drain thoroughly. Recrystallise from ethanol methylated spirit should not be used, as it contains sufficient water to cause partial hydrolysis back to benzaldehyde and ammonia. Hydrobenzamide is obtained as colourless crystals, m.p. 101° (and not 110° as frequently quoted) yield, 4 g. 

Gently warm a mixture of 32 g. (32 ml.) of ethyl acetoacetate and 10 g. of aldehyde-ammonia in a 400 ml. beaker by direct heating on a gauze, stirring the mixture carefully with a thermometer. As soon as the reaction starts, remove the heating, and replace it when the reaction slackens, but do not allow the temperature of the mixture to exceed 100-no the reaction is rapidly completed. Add to the mixture about twice its volume of 2A -hydrochloric acid, and stir the mass until the deposit either becomes solid or forms a thick paste, according to the quality of the aldehyde-ammonia employed. Decant the aqueous acid layer, repeat the extraction of the deposit with more acid, and again decant the acid, or filter off the deposit if it is solid. Transfer the deposit to a conical flask and recrystallise it twice from ethanol (or methylated spirit) diluted with an equal volume of water. The i,4-dihydro-collidine-3,5-dicarboxylic diethyl ester (I) is obtained as colourless crystals, m.p. 130-131°. Yield 12 5 g,... 

Succinamide. Add 5 g. (4-8 ml.) of dimethyl succinate to 25 ml. of concentrated ammonia solution (sp. gr. 0-88) in a 100 ml. conical flask. Cork the flask and shake the contents for a few minutes aUow to stand for 24 hours with occasional shaking. Filter off the crystals of succinamide, and wash with a Uttle cold water. RecrystaUise from a little hot water. Dry in the steam oven and determine the m.p. The yield is 3-5 g. Pure succinamide melts at 254° with decomposition. 

To recover the free base, dissolve the hydrochloride in the minimum volume of boiling alcohol, add concentrated ammonia solution dropwise until a clear solution results and the blue colour has become fight brown. Add water carefully untU a cloudiness appears, warm on a water bath untU the cloudiness just disappears, and allow to cool. Yellow crystals of p-amino-azobenzene separate on coofing. 

Nicotinamide. Place 50 g. of pure ethyl nicotinate (Section V,23) in a 350 ml. bolt-head flask and add 75 ml. of concentrated aqueous ammonia saturated at 0°. Keep the flask loosely stoppered for 18 hours, after w)iich time the lower layer generally dissolves on shaking. Saturate the solution with ammonia and allow it to stand for a further 4 hours. Repeat the saturation with ammonia crystals of the amide commence to appear in the solution. Evaporate to drjmess in a dish on the steam bath and dry at 120°. The yield of nicotinamide, m.p. 130°, is usuallj quantitative. 

In a 500 ml. Pyrex round-bottomed flask, provided with a reflux condenser, place a mixture of 40 g. of freshly-distUled phenylhydrazine (Section IV.89) and 14 g. of urea (previously dried for 3 hours at 100°). Immerse the flask in an oil bath at 155°. After about 10 minutes the urea commences to dissolve accompanied by foaming due to evolution of ammonia the gas evolution slackens after about 1 hour. Remove the flask from the oil bath after 135 minutes, allow it to cool for 3 minutes, and then add 250 ml. of rectified spirit to the hot golden-yellow oil some diphenylcarbazide will crystallise out. Heat under reflux for about 15 minutes to dissolve the diphenylcarbazide, filter through a hot water funnel or a pre-heated Buchner fuimel, and cool the alcoholic solution rapidly in a bath of ice and salt. After 30 minutes, filter the white crystals at the pump, drain well, and wash twice with a little ether. Dry upon filter paper in the air. The yield of diphenylcarbazide, m.p. 171 °, is 34 g. A further 7 g. may be obtained by concentrating the filtrate under reduced pressure. The compound may be recrystallised from alcohol or from glacial acetic acid. 

The dibromohydrate is first produced, and treatment with ammonia gives the free base, which after recryslallization in nitrobenzene gives brown crystals (m.p. 215°C). The picrate decomposes around 254°C. 

The action of ammonia on N-(aryl-i,3-oxathiol-2-ylidine) tertiary im-inium salts (254) yields linear intermediates (255) that cyclize to 2-amino-4-phenyl thiazoles (256) on crystallization from acetic acid (Scheme 129) (730). 

Acetaldehyde can be isolated and identified by the characteristic melting points of the crystalline compounds formed with hydrazines, semicarbazides, etc these derivatives of aldehydes can be separated by paper and column chromatography (104,113). Acetaldehyde has been separated quantitatively from other carbonyl compounds on an ion-exchange resin in the bisulfite form the aldehyde is then eluted from the column with a solution of sodium chloride (114). In larger quantities, acetaldehyde may be isolated by passing the vapor into ether, then saturating with dry ammonia acetaldehyde—ammonia crystallizes from the solution. Reactions with bisulfite, hydrazines, oximes, semicarb azides, and 5,5-dimethyl-1,3-cyclohexanedione [126-81 -8] (dimedone) have also been used to isolate acetaldehyde from various solutions. 

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