Hydrochloric acid melting point

The hydrochloride can be obtained from the base by the addition of hydrochloric acid. Melting point 188—190°C (from acetonitrile). 

Butyl lithium (10 ml, 1.64 mol in hexane) was added under nitrogen to a stirred suspension of triphenyl-2-pyrrolidinoethylphosphonium bromide (7.2 g) in dry toluene (75 ml). After 0.5 h, ((E)-3-(6-(4-toluoyl)-2-pyridyl)acrylate, vide supra, (4.8 g) in toluene (50 ml) was added. The suspension, initially orange, became deep purple, then slowly faded to yellow during 2 h heating at 75°C. The cooled solution was diluted with ether (150 ml) and treated with hydrochloric acid (50 ml, 2 mol). The aqueous phase was separated, washed with ether, and basified with potassium carbonate (ice) and extracted with ether. The mixture of isomeric esters obtained by evaporation was dissolved in ethanol (100 ml) containing sodium hydroxide solution (20 ml, 1 mol) and partially evaporated on the steam bath under reduced pressure for 5 min. The residual aqueous solution was neutralized with sulfuric acid (20 ml, 0.5 mol) and evaporated to dryness. The solid residue was extracted with hot isopropanol (3x50 ml) and the extracts were concentrated until crystallization commenced. The (E)-3-(6-(3-pyrrolidino-l-(4-tolyl)prop-l-(E)-enyl)-2-pyridyl)acrylic acid, melting point 222°C (dec. recrystallization from isopropanol) was obtained. 

A solution of methyl 3-(3-trifluoromethylphenyl)-4-amino-5-isothiazolecarboxylate and potassium hydroxide in methanol was heated at reflux for 6 h. The reaction mixture was then poured into ice containing 12 N aqueous hydrochloric acid. The free acid precipitated from the acidic solution, and after all of the ice had melted, the aqueous acidic mixture was filtered. The precipitate was crystallized from ethanol and water to provide 3-(3-trifluoromethylphenyl)-4-amino-5-isothiazolecarboxylic acid, melting point 179°-180°C. Yield 80%. 

A mixture of methyl 6-chloro-3,4-dihydro-4-methyl-3-oxo-2H-l,4-benzoxazine-8-carboxylate, ethanol and 4% aqueous potassium hydroxide solution is refluxed with heating. The resultant solution is cooled and water is added thereto followed by filtration. The filtrate is made acid with concentrated hydrochloric acid. The precipitated crystals are collected by filtration, washed with water and dried, and then recrystallized from ethanol to give 6-chloro-3,4-dihydro-4-methyl-3-oxo-2H-l,4-benzoxazine-8-carboxylic acid, melting point 241°-243°C. 

After cooling of the medium, 120 ml of water containing 11.6 g of sodium carbonate and ether are introduced, the aqueous phase is decanted and washed with ether, whereupon the aqueous phase is acidified to a pH of 1 with 50% hydrochloric acid. The desired product is extracted with ethyl acetate. After elimination of the extraction solvent 31.5 g of the 4-(3,4,5-trimethoxyphenyl)-4-oxo-2-hydroxy butanoic acid, melting point 119°-120°... 

A solution of 0.197 mole of diethyl (N,N -(2-chloro-5-cyano-m-phenylene) dioxamate in 750 ml of methylene chloride is extracted with 465 ml of 1 N sodium hydroxide. The aqueous phase is separated and stirred for 20 min at room temperature. The solution is acidified with dilute hydrochloric acid. The precipitate is removed by filtration and washed with water. There is obtained 59.1 g (96%) of N,N -(2-chloro-5-cyano-m-phenylene)dioxamic acid, melting point 212°C (dec.). 

Hydroxy-6-methoxybenzaldehyde (16.875 g, 0.111 M), ethyl 5-bromopentanoate (23.25 g, 17.6 ml, 0.111 M), anhydrous potassium carbonate (16.5 g), sodium iodide (0.675 g) and 95% ethanol (150 ml) were refluxed with stirring (16 hours). The cooled reaction mixture was filtered and the solid washed well with ethanol. The filtrate was evaporated to dryness and the residue partitioned between ether and water. The ethereal layer was separated and washed with 2 N sodium hydroxide solution, water, dried (sodium sulfate) and evaporated. The residue was dissolved in 95% ethanol (300 ml) and 0.66 N sodium hydroxide solution (450 ml) and stirred at ambient temperature (4 hours). The reaction mixture was evaporated to half volume and diluted with water. The mixture was extracted once with ether and the aqueous layer acidified with concentrated hydrochloric acid with cooling. The crystalline solid formed was filtered off and washed well with water. Recrystallisation from ethyl acetate-petrol gave 5-(2-formyl-3-methoxyphenoxy)pentanoic acid, melting point 99-101°C. 

To a suspension of 3-(4-bromo-2-fluorobenzyl)-7-chloro-l,2,3,4-tetrahydro-2,4-dioxoquinazoline in N,N-dimethylformamide was added sodium hydride (60% in mineral oil) with stirring at 0°C and the mixture was stirred for 15 min at the same temperature. To this mixture was added ethyl bromoacetate and the mixture was stirred for 1 h at room temperature. The reaction mixture was poured into diluted hydrochloric acid and extracted with ethyl acetate. The extract was washed with brine, dried and evaporated to give a residue. Thus obtained product was purified by recrystallization from isopropyl ether to give 2-[3-(4-bromo-2-fluorobenzyl)-7-chloro-l,2,3,4-tetrahydro-2,4-dioxoquinazolin-l-yl]acetic acid melting point 223°-224°C. 

A mixture of 40.6 g of the ethyl 1,3-dihydro-2-oxo-3-benzyl-lH-benzimidazol-1-butanoate and 400 ml of 1 N methanolic sodium hydroxide was refluxed for 3 h under an inert atmosphere and was then concentrated to 0.5 its value and was poured into 1 L of iced water. The pH was adjusted to 2 by addition of concentrated hydrochloric acid and the mixture was vacuum filtered. The product was washed and dried to obtain 35.2 g of 1,3-dihydro-2-oxo-3-benzyl-lH-benzimidazol-l-butanoic acid, melting point 168°C (crystallization from ethyl acetate). 

Drop 1 g. of sodium into 10 ml. of ethyl alcohol in a small flask provided with a small water condenser heat the mixture until all the sodium has dissolved. Cool, and add 1 g. of the ester and 0-5 ml. of water. Frequently the sodium salt of the acid will be deposited either at once or after boiling for a few minutes. If this occurs, filter oflF the solid at once, wash it with a little absolute ethyl alcohol (or absolute methylated spirit), and convert it into the p-bromophenacyl ester, p-nitro-benzyl ester or S-benzyl-tso-thiuronium salt (for experimental details, see Section 111,85). If no solid separates, continue the boiling for 30-60 minutes, boil oflF the alcohol, allow to cool, render the product just neutral to phenolphthalein with dilute sulphuric or hydrochloric acid, convert the sodium salt present in solution into a crystalline derivative (Section 111,85), and determine its melting point. 

Lithium Chloride. Lithium chloride [7447- 1-8], LiCl, is produced from the reaction of Hthium carbonate or hydroxide with hydrochloric acid. The salt melts at 608°C and bods at 1382°C. The 41-mol % LiCl—59-mol % KCl eutectic (melting point, 352°C) is employed as the electrolyte in the molten salt electrolysis production of Hthium metal. It is also used, often with other alkaH haHdes, in brazing flux eutectics and other molten salt appHcations such as electrolytes for high temperature Hthium batteries. 

Camphene hydrochloride, Cj(,H gHCl, is prepared by passing dry hydrochloric acid into an alcoholic solution of camphene. When re-ctystallised from an alcoholic solution containing excess of hydrochloric acid, it melts at 155° (or possibly a few degrees lower).- Melting-points from 149° to 165° have been recorded for this compound, but the products examined were probably not in a state of purity. 

Sehlogl has shown that para-aminophenylglycine, para-amino-phenyloxamic acid, and para-aminoacetanilide form compounds with aldehydes, which have sharp melting-points and are suitable for the characterisation of aldehydes. With p-aminophenylglycine condensation takes place when the glycine, mixed with alcohol and the aldehyde in question, is warmed. For the purpose of condensing with p-aminophenyloxamic acid and with p-aminoacetaldehyde the alcoholic suspension of the amino-hody is acidulated slightly with hydrochloric acid and the solution is warmed after the aldehyde has heen added. This method yields the hydrochloride of the condensation products. 

The hydrochloride is prepared by dissolving the base in the minimum amount of acetone and adding a solution of hydrochloric acid in ether until the pH is acid. The hydrochloride which has precipitated is filtered off and is recrystallized twice from acetone, melting point 116°C. 

About 3 grams of 0-methylcholine chloride are stirred at room temperature with an excess of phosgene dissolved in 50 grams of chloroform, for about 2 hours. Excess phosgene and hydrochloric acid are removed by distillation under vacuo. Additional chloroform is added to the Syrup and the mixture is poured into excess ammonia dissolved in chloroform and cooled in solid carbon dioxide-acetone. The solid is filtered and extracted with hot absolute alcohol. The solid in the alcohol is precipitated with ether, filtered, and recrystallized from isopropanol. The carbaminoyl-0-methylcholine chloride obtained has a melting point of about 220°C. 

B.Bg (0.15 mol) of 4-phenylbenzophenoneare dissolved in 200 ml of ethanol and 3 g (0.075 mol) of sodium borohydride are added. After heating for 15 hours under reflux, and allowing to cool, the reaction mixture is hydrolyzed with water containing a little hydrochloric acid. The solid thereby produced is purified by recrystallization from ethanol, 36 g (B9% of theory) of (biphenyl-4-yl)-phenyl-carbinol [alternatively named as diphenyl-phenyl carblnol or a-(biphenyl-4-yl)benzylalcohol] of melting point 72°-73°C are obtained. 

To produce the dihydrochloride, the free base is dissoived in 110 cc of absolute alcohol, 9.6 g of dry hydrochloric acid dissolved In 35 cc of alcohol are added, followed by 2.8 cc of water. The dihydrochloride precipitates. Is centrifuged, washed, and dried at 40°C. It was a solid white material having a melting point of 134°-135°C. 

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