N Hydrochlorid

Chlor-hydrat, n. hydrochloride chlorine hydrate. -hydrin, n. chlorohydrin. 

The thus yielded active fraction, about 200 ml, was neutralized with sodium hydroxide, concentrated to about 15 ml in vacuo, separating the precipitated inorganic salts therefrom. After decolorization with active carbon, 150 ml of methanol was added, the mixture was allowed to stand overnight at 5°C and the precipitate was collected by filtration. The precipitate was washed with methanol and dried in vacuo to yield crude tuberactinomycin-N hydrochloride (yield, 3.07 g purity, 71 S% recovery, 62%). 

Gastric acidity Ketoconazole requires acidity for dissolution and absorption. In achlorhydria, dissolve each tablet in 4 ml aqueous solution of 0.2 N hydrochloride. Use a glass or plastic straw to avoid contact with teeth. Follow with a glass of water. 

Treatment of ethyl 2-azidobutanoate with catalytic quantities of lithium ethoxide in tetrahydrofuran leads to the evolution of nitrogen. On quenching the resulting solution with 3 N hydrochloride acid, ethyl 2-oxobutanonate is isolated in 86% yield. Suggest a mechanism for this process. 

Dissolve 7.50 g glycine (aminoacetic acid, glycocoll) in 500 ml ddH20. Adjust the wanted pH by using 0.1 N hydrochloride acid, then fill up to 1000 ml. 

A. 2-Bromo-2-cyclopentenone. In a well-ventillated hood, a solution of 18.98 g (231.2 mmol) of 2-cyclopentenone (Note 1) in 150 mL of carbon tetrachloride is added to a 1-L, three-necked, round-bottomed flask fitted with a mechanical stirrer, thermometer, and an addition funnel. The solution is chilled to 0°C with an ice bath and a solution of 40.5 g (253.4 mmol, 13.0 mL) of bromine in 150 mL of carbon tetrachloride is added dropwise during 1 hr. Then a solution of 35.1 g (346.8 mmol, 48.3 mL) of triethylamine in 150 mL of carbon tetrachloride is added dropwise over 1 hr with vigorous stirring while the reaction is held at 0°C. Stirring is continued for an additional 2 hr at room temperature the resulting dark suspension is filtered with suction and the filter cake washed with carbon tetrachloride. The filtrate and washings are combined and washed with two 100-mL portions of 2 N hydrochloride acid, one 100-mL portion of saturated sodium bicarbonate solution, one 100-mL portion of water, and one 100-mL portion of saturated sodium chloride solution. The resultant solution is dried over anhydrous magnesium sulfate, filtered, and the solvent removed under reduced pressure. Distillation of the resultant oil (69-78°C, 1.0 mm) afforded 23.7 g (147.2 mmol, 64%) (Note 2) of a white crystalline solid (mp 36-37°C, lit.2 mp 39-39.5°C) (Note 3). 

Eight known bases were isolated from this plant, namely, erysopine, erythraline, erythramine, erysodine, erysotrine, erythratine, N,N-dimethyltryptophan, and hypaphorine. In addition three alkaloids, not previously known to occur naturally, were isolated, namely, N-norprotosinomenine (CigHaiO N hydrochloride, mp 242-244° [a] +18°) (74), protosinomenine (picrolonate, mp 172-174°) (75) which was methylated to laudanosine (mp 83-85°), and j8-erythroidine (76) (92). 

Using 0.1 % N hydrochloride to adjust the pH of the water bath from 4.5-7.0, a pH of 5.0 produced the most primorida and mature mushrooms. 

The conversion of the extrudate was determined by titration of the unreacted isocyanate groups in toluene. Between 0.5 and 0.8 gram of the sample was dissolved in 24 ml of toluene. To this solution, 25ml of a 0.1 N butylamine solution in toluene was dosed, after which the mixture was allowed to react for 20 min. Afterwards, 100 ml of isopropyl alcohol and five drops of 0.1 % bromophenol blue were added. The solution was then titrated with a 0.1 N hydrochloride solution. Subsequently the same procedure was repeated without any sample for eomparison. 

SchifT s bases A -Arylimides, Ar-N = CR2, prepared by reaction of aromatic amines with aliphatic or aromatic aldehydes and ketones. They are crystalline, weakly basic compounds which give hydrochlorides in non-aqueous solvents. With dilute aqueous acids the parent amine and carbonyl compounds are regenerated. Reduction with sodium and alcohol gives... 

Aminoazobenzene is a very weak base, and consequently it will not form salts with weak organic acids, such as acetic acid, although it will do so with the strong mineral acids, such as hydrochloric acid. Aminoazobenzene is a yellowish-brown compound, whilst the hydrochloride is steel blue. The colour of the latter is presumably due to the addition of the proton to the phenyl-N-atom, the cation thus having benzenoid and quinonoid forms ... 

Into a 500 ml. three-necked flask, provided with a mechanical stirrer, a gas inlet tube and a reflux condenser, place 57 g. of anhydrous stannous chloride (Section 11,50,11) and 200 ml. of anhydrous ether. Pass in dry hydrogen chloride gas (Section 11,48,1) until the mixture is saturated and separates into two layers the lower viscous layer consists of stannous chloride dissolved in ethereal hydrogen chloride. Set the stirrer in motion and add 19 5 g. of n-amyl cyanide (Sections III,112 and III,113) through the separatory funnel. Separation of the crystalline aldimine hydrochloride commences after a few minutes continue the stirring for 15 minutes. Filter oflF the crystalline solid, suspend it in about 50 ml. of water and heat under reflux until it is completely hydrolysed. Allow to cool and extract with ether dry the ethereal extract with anhydrous magnesium or calcium sulphate and remove the ether slowly (Fig. II, 13, 4, but with the distilling flask replaced by a Claisen flask with fractionating side arm). Finally, distil the residue and collect the n-hexaldehyde at 127-129°. The yield is 19 g. 

The modified procedure involves refluxing the N-substituted phthaUmide in alcohol with an equivalent quantity of hydrazine hydrate, followed by removal of the alcohol and heating the residue with hydrochloric acid on a steam bath the phthalyl hydtazide produced is filtered off, leaving the amine hydrochloride in solution. The Gabriel synthesis has been employed in the preparation of a wide variety of amino compounds, including aliphatic amines and amino acids it provides an unequivocal synthesis of a pure primary amine. 

Group IV. The student should remember that the hydrochlorides of some bases are sparingly soluble in cold water and should therefore not be misled by an apparent insolubility of a compound (containing N) in dilute hydrochloric acid. The suspension in dilute hydrochloric acid should always be filtered and the filtrate made alkaline. A precipitate will indicate that the compound should be placed in Group IV if no precipitate is formed, the compound is relegated to Group VII. 

B. Mix 1 drop or several small crystals (ca. 0 05 g.) of the compound with 1 ml. of 0-5 V hydroxylamine hydrochloride in 95 per cent, ethanol and add 0-2 ml ot aqueous sodium hydroxide. Heat the mixture to boiling and, after the solution has cooled slightly, add 2 ml. of N hydrochloric acid. If the solution is cloudy, add 2 ml. of 95 per cent, ethyl alcohol. Observe the colour produced when I drop of 6 per cent, ferric chloride solution is added. If the resulting colour does not persist, continue to add the reagent dropwise until the observed colour pervades the entire solution. Usually only 1 drop of the ferric chloride solution is necessary. Compare the colour with that produced in test. 4. A positive test will be a distinct burgundy or magenta colour as compared with the yellow colour observed when the original compound is tested with ferric chloride solution in the presence of acid. 

Separations based upon differences in the chemical properties of the components. Thus a mixture of toluene and anihne may be separated by extraction with dilute hydrochloric acid the aniline passes into the aqueous layer in the form of the salt, anihne hydrochloride, and may be recovered by neutralisation. Similarly, a mixture of phenol and toluene may be separated by treatment with dilute sodium hydroxide. The above examples are, of comse, simple apphcations of the fact that the various components fah into different solubihty groups (compare Section XI,5). Another example is the separation of a mixture of di-n-butyl ether and chlorobenzene concentrated sulphuric acid dissolves only the w-butyl other and it may be recovered from solution by dilution with water. With some classes of compounds, e.g., unsaturated compounds, concentrated sulphuric acid leads to polymerisation, sulphona-tion, etc., so that the original component cannot be recovered unchanged this solvent, therefore, possesses hmited apphcation. Phenols may be separated from acids (for example, o-cresol from benzoic acid) by a dilute solution of sodium bicarbonate the weakly acidic phenols (and also enols) are not converted into salts by this reagent and may be removed by ether extraction or by other means the acids pass into solution as the sodium salts and may be recovered after acidification. Aldehydes, e.g., benzaldehyde, may be separated from liquid hydrocarbons and other neutral, water-insoluble hquid compounds by shaking with a solution of sodium bisulphite the aldehyde forms a sohd bisulphite compound, which may be filtered off and decomposed with dilute acid or with sodium bicarbonate solution in order to recover the aldehyde. 

Footnote 4 - The solubility of Ammonium Chloride in absolute Ethanol is 0.6g/100g at 15C. The solubility in n-Butyl Alcohol is neglible, even at its boiling point. If you use n-Butyl Alcohol, you will only need to perform 3 reflux/filter operations to obtain sufficiently pure Methylamine Hydrochloride. 

To illustrate the specific operations involved, the scheme below shows the first steps and the final detachment reaction of a peptide synthesis starting from the carboxyl terminal. N-Boc-glycine is attached to chloromethylated styrene-divinylbenzene copolymer resin. This polymer swells in organic solvents but is completely insoluble. ) Treatment with HCl in acetic acid removes the fert-butoxycarbonyl (Boc) group as isobutene and carbon dioxide. The resulting amine hydrochloride is neutralized with triethylamine in DMF. 

Aminothiazolium hydroxide inner salts (2) (X = NR) are only known as N-phenyl (29) or acyl derivatives. (6. 34) or as hydrochlorides (35). 

The 5-amino-THISs are very strong bases (35). The hydrochlorides, therefore, have not yet been deprotonized successfully. However, the decreased basicity of the N-acylated derivatives makes these readily accessible from their hydrochlorides (Scheme 28). 

Benzylidenehydrazinoselenazoies are stable to acids and do not decompose with time. The isopropylidene homologs are only stable in the form of the hydrochloride, and they can undergo acid hydrolysis, thus providing a convenient pathway to the free hydrazine (32). Hydrolysis is carried out w ith hot 2 N hydrochloric acid, which, after recooling and filtration, leads to 2-hydrazinoselenazole hydrochloride, yielding the free base upon neutralization (Scheme 19, Table X-6). 

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