Benzene solution aqueous

Place a mixture of 25 5 g. of n-valerio acid (Sections 111,83 and 111,84), 30 g. (37 -5 ml.) of dry n-propyl alcohol, 50 ml. of sodium-dried benzene and 10 g. (5-5 ml.) of concentrated sulphuric acid in a 250 ml. round-bottomed flask equipped with a vertical condenser, and reflux for 36 hours. Pour into 250 ml. of water and separate the upper layer. Extract the aqueous layer with ether, and add the extract to the benzene solution. Wash the combined extracts with saturated sodium bicarbonate solution until effervescence ceases, then with water, and dry with anhydrous magnesium sulphate. Remove the low boiling point solvents by distillation (use the apparatus of Fig. II, 13,4 but with a Claisen flask replacing the distilling flask) the temperature will rise abruptly and the fi-propyl n-valerate will pass over at 163-164°. The yield is 28 g. 

Sulphonamides. Mix together 1 0 g. of the dry acid or 1 - 2 g. of the anhydrous salt with 2 5 g. of phosphorus pentachloride f and heat under a reflux condenser in an oil bath at 150° for 30 minutes. Cool the mixture, add 20 ml. of dry benzene, warm on a steam bath and stir the solid mass well to extract the sulphonyl chloride filter. Add the benzene solution slowly and with stirring to 10 ml. of concentrated ammonia solution. If the sulphonamide precipitates, separate it by filtration if no solid is obtained, evaporate the benzene on a steam bath. Wash the sulphonamide with a little cold water, and recrystallise from water, aqueous ethanol or ethanol to constant m.p. 

Transfer 30 g. of the hydrochloride to a 500 ml. separatory funnel, add 100 ml. of water and shake until a thin paste of uniform consistency is obtained add 10 per cent, aqueous sodium hydroxide solution in the cold with shaking until the whole mass has become bright green (the colour of the free base) and the mixture has an alkaUne reaction. Extract the free base by shaking with two 60 ml. portions of benzene (1). Dry the combined benzene extracts with a Uttle anhydrous potassium carbonate, and filter into a distiUing flask fitted with a water condenser. Distil off about half of the benzene, and pour the residual hot benzene solution into a beaker. Upon cooUng, the p-nitrosodimethylaniUne erystallises in deep green leaflets. Filter these off and dry them in the air. The yield of p-nitrosodimethylaniUne, m.p. 85°, from the hydrochloride is almost quantitative. 

I) The steam distillation may be omitted, if desired, by utilising the following method of purihcation. Allow the reaction mixture to cool, decant the aqueous layer and dissolve the residue in about 150 ml. of benzene. Wash the benzene solution with water, I per cent, sodium hydroxide solution, and finally with water dry with anhydrous magnesium sulphate, distil oft the benzene on a water bath, and distil the residue under diminished pressure. 

Benzenetetrol. 1,2,3,5-Tetrahydroxybenzene (64) forms needles (mp 165°C) from water. The compound is easily soluble ia water, alcohol, and ethyl acetate and is iasoluble ia chloroform and benzene. In aqueous potassium bicarbonate solution sparged with carbon dioxide,... 

Tri-n-octylphosphine oxide [78-50-2] M 386.7, m 59.5-60°, pK jt <0. Mason, McCarty and Peppard [J Inorg Nuclear Chem 24 967 7962] stirred an O.IM solution in benzene with an equal volume of 6M HCl at 40° in a sealed flask for 48h, then washed the benzene solution successively with water (twice), 5% aq Na2C03 (three times) and water (six times). The benzene and water were then evaporated under reduced pressure at room temperature. Zingaro and White [J Inorg Nucl Chem 12 315 7960] treated a pet ether solution with aqueous KMn04 (to oxidise any phosphinous acids to phosphinic acids), then with sodium oxalate, H2SO4 and HCl (to remove any manganese compounds). The pet ether solution was slurried with activated alumina (to remove phosphinic acids) and recrystd from pet ether or cyclohexane at -20°. It can also be crystd from EtOH. 

Molecular bromine is believed to be the reactive brominating agent in uncatalyzed brominations. The brominations of benzene and toluene are first-order in both bromine and the aromatic substrate in trifluoroacetic acid solution, but the rate expressions become more complicated when these reactions take place in the presence of water. " The bromination of benzene in aqueous acetic acid exhibits a first-order dependence on bromine concentration when bromide ion is present. The observed rate is dependent on bromide ion concentration, decreasing with increasing bromide ion concentration. The detailed kinetics are consistent with a rate-determining formation of the n-complex when bromide ion concentration is low, but with a shift to reversible formation of the n-complex... 

Androst-4-ene-3,17,19-trione (0.23g) is added to a precooled solution of 0.23 g of potassium hydroxide in a mixture of 1 ml of water and 5 ml of methanol. The reaction mixture is stirred at 5-10° under nitrogen for 3 hr, diluted with benzene (30 ml) and washed with water (2 x 10 ml). The aqueous layer is reextracted with benzene and the benzene solution dried and evaporated. The crude crystalline product is filtered through 8 g of Merck silicagel and eluted with benzene-ethyl acetate (9 1) to yield 0.19 g of 19-norandrostenedione (88%) mp 169-171° 141° (CHCI3). 

Hydroxy-5a-pregn-l-ene-3,20-dione (44). To a solution of 7.7 g (15.6 mmoles) of the nitrone (43) in 300 ml of benzene is added 500 ml of 2 A hydrochloric acid, whereupon the deep-red benzene solution immediately turns green. The resulting mixture is stirred for 12 hr and the layers are then separated. The aqueous layer is extracted with three 300-ml portions of benzene the combined benzene layers are washed with 2 N hydrochloric acid and with water, and then dried over sodium sulfate. The benzene is evaporated under reduced pressure to give 4.8 g (93 %) of the diosphenol (44). 

Fullerols, C6o(OH) (n = 24-26), can be synthesized directly by aerobic oxidation of a benzene solution of Qq using an aqueous solution of NaOH containing a few drops of BimNOH as the most efficient catalyst the deep violet benzene solution rapidly decolorizes and a brown sludge precipitates further reaction with more water over a period of 10 h gives a clear red-brown solution from which the... 

The dihydrochloride is converted into monohydrochloride by dissolving 26.36 g (0.066 mol) of dihydrochloride into 158 cm of water, adding drop by drop a suitable amount (0.066 mol) of caustic soda (1 N), evaporating the aqueous solution to dryness, drying by means of benzene, filtering the formed sodium chloride (3.8 g) and crystallizing the cooled obtained benzene solution. 22.6 g (95%) of monohydrochloride are obtained, MP 120° to 121 t. 

The aqueous solutions resulting from the washing are also extracted with ether, and the ether portions are added to the main ether-benzene solution. 

A solution of 1-piperazino ethyl acetate (Q2 mol) in benzene (300 ml) is treated with 3,4.5-trimethoxy cinnamoyl chloride (0,2 mol) in the presence of sodium bicarbonate (0.3 mol). After contacting for one hour at room temperature, the mixture is refluxed for a further hour. The benzene solution is then treated with an aqueous solution of sodium bicarbonate. After evaporation of the solvent, a solid product is obtained which is recrystallized from isopropyl ether. Melting point = 96°C. This base, when treated with hydrochloric acid, gives a hydrochloride having a melting point of 200°C with decomposition. By the action of malaic acid the acid maleate is obtained, having a melting point of 130°C. 

Preparation of Alkaloid Mixture 50 ml of the concentrated benzene solution, obtained as described was rapidly stirred, and a saturated solution of hydrogen chloride in ether added to the concentrated benzene solution until no more precipitate was obtained. The resulting precipitate was recovered by filtration and comprised the crude hydrochlorides of the extracted alkaloids and the hydrochloride of any unrecovered triethylamine. This material was dried by heating at a temperature of about 75°C for 6 hours, the crude, dried precipitate ground with 50 ml of isopropanol and to this slurry was added 1,000 ml of water. The resulting mixture was filtered. To the clear filtrate, cooled to 5°C, there was slowly added with rapid stirring, a 10% aqueous solution of ammonium hydroxide, until complete precipitation was accomplished. The precipitate was filtered off, washed with water and dried by heating at about 75°C for 6 hours. 

A solution of 50 grams of N-(a-methylhomoveratryl)-3-methoxy-4-ethoxyphenylacetamide, prepared as set out above, in 200 cc of benzene, is treated with 8 cc of phosphorus oxychloride. The mixture is refluxed for about 3 hours, cooled and then is shaken with a solution composed of 15 grams of sodium hydroxide dissolved in 60 cc of water. The aqueous layer is removed, and the benzene solution is washed with water. The washed benzene solution is dried over anhydrous magnesium sulfate, filtered and evaporated to dryness. The low-melting solid residue is 6,7-dimethoxy-3-methyl-1-(3 -methoxy-4 -ethoxybenzyl)-dihydroisoquinoline base. 

The solvent is evaporated in vacuo, the residue is dissolved in anhydrous acetone and the hydrochloride formed is filtered. The corresponding base is liberated by treating the aqueous solution of this hydrochloride with an excess of potassium carbonate. A benzene extraction is effected and the benzene solution of the base is dried over potassium carbonate. 

A mixture of 0.1 mol of N-mono-1-p-chlorobenzohydrylpiperazine and 0.1 mol of 1-chloro-2-(2-hydroxy-ethoxy)-ethane is heated for 3 hours to 150°C. The mass is then taken up in 100 ml of benzene and 100 ml of a 10% aqueous solution of NaOH decanting takes place, and the benzene solution is washed with water and the solvent is evaporated. Vacuum distilling of the residue yields 1-p-chlorobenzohydryl-4-[2-(2-hydroxy-ethoxy)-ethyl]-piperazine, BP 220 C/0.5 mm Hg. 

A mixture of 1B g of 1 -acetamido-3,5-dimethvladamantane, 3B g of sodium hydroxide, and 300 ml of diethylene glycol was refluxed for a period of 6 hours. The reaction product mixture was cooled and poured onto about IfiQQ ml of crushed Ice. The basic solution thus obtained was extracted five times with 250-ml portions of benzene and the aqueous layer was discarded. The combined benzene extracts were dried over sodium hydroxide and the dried benzene solution concentrated in vacuo to give a crude oil weighing 14 g and having np =... 

Sodium (9.6 parts) was dissolved in butanol (192 parts) and di-n-butyl ethyl 1 -methyl-n-butylmalonate (62,B parts) and urea (14.4 parts) were added to the warm solution with agitation. The mixture was then heated to reflux temperature in three quarters of an hour and maintained for 2 hours. The reaction mass was kept, water (150 parts) added, the aqueous portion separated, and the butanol layer extracted with water (3 x 50 parts). The combined aqueous extracts were then given 3 small extractions with benzene, the aqueous liquors separated, charcoaled,filtered and precipitated with concentrated hydrochloric acid (acid to congo-paper). The solid was collected, washed with water, dissolved in N-sodium hydroxide and reprecipitated with carbon dioxide. On recrystallization, from aqueous alcohol, the pentobarbitone was obtained. 

B) Preparation of 2-(Hydroxyiminomethyl)-1-Methyl Pyridinium Chloride An aqueous solution of 15 ml of 1-methyl-2-picolinium chloride having a concentration of 477 mg/ml Is covered with 50 ml of benzene in an atmosphere of nitrogen and cooled to below 10°C. An aqueous solution of sodium hydroxide is added dropwise and the mixture is stirred for 5 minutes and allowed to stratify. The aqueous phase Is then drawn off and the benzene solution is added slowly to a solution of 3 ml of nitrosyl chloride in 175 ml of benzene containing 0.5 ml of dimethyl formamide at about 10°C in an atmosphere of nitrogen with good agitation. The mixture is then stirred for 1.5 hours and then extracted with four... 

A mixture of the arylsulfonyl chloride (5 mmol), benzene (2.56 mol), NaN3 (5 mmol), NaHCO, (20 mmol), and methyltrioctylammonium chloride (0.5 mmol), under N2 in an autoclave, was stirred al 40 C for 3 h. The mixture was then heated slowly to 125 C and maintained at this temperature for another 3 h, during which time the pressure in the vessel rose to 31 -54 atm. The mixture was allowed to cool and the autoclave was depressurized. The residual mass was filtered, and the residue washed thoroughly with cold H20. The benzene solution was separated from the aqueous filtrate, dried, and evaporated to give the crude product as a reddish yellow mass which was purified by column chromatography (neutral alumina, hexane/ benzene 3 2). The 1-(arylsulfonyl)-l//-azepines 16 were crystallized from light petroleum ether (bp 60-80 LC). 

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