Aluminum , diethyl-, sulfate

Nitrogen Dioxide Aluminum Sodium Sulfate SAS 10545-99-0 105-53-3 Nitrogen Tetraoxide Sulfur Dichloride Diethyl Malonate... 

The mixture is cooled and the excess of lithium aluminum hydride is decomposed with cracked ice. The water layer is separated and washed with diethyl ether. The combined ether extracts are dried over anhydrous magnesium sulfate and the solvent is removed by distillation under reduced pressure. Yield, 8.8 g boiling point, 160°C to 165°C/0.1 mm Hg. 

R)-aluminum-lithium-BINOL complex (0.024 g, 0.04 mmol) was dissolved in toluene (0.4 ml), and to this solution was added dimethyl phosphite (0.044 g, 0.4 mmol) at room temperature the mixture was stirred for 30 min. Benzaldehyde (0.042 g, 0.4 mmol) was then added at -40°C. After having been stirred for 51 h at -40°C, the reaction mixture was treated with 1 N hydrochloric acid (1.0 ml) and extracted with ethyl acetate (3 x 10 ml). The combined organic extracts were washed with brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by flash chromatography (silica, 20% acetone/hexane) to give the diethyl (S)-a-hydroxybenzylphosphonate (78 mg, 90%) with 85% enantiomeric excess as a colorless solid of mp 86 to 87°C. 

Aluminum foil, Iodine powder. Carbon disulfide, 1,4,6,9-Tetrabromodiamantane, Sodium bisulfite. Hydrochloric acid. Methanol, Acetonitrile, Acetone, Sodium hydroxide. Magnesium sulfate. Potassium permanganate. Toluene Methylene chloride, 2-Bromomethanol, Trioxane, Aluminum chloride. Magnesium sulfate, Nitroform, Acetone, Sodium bicarbonate. Hexane, Silver nitrate. Acetonitrile 1,2-Dichloroethane, HexamethyldisUane, Iodine, Cyclohexane, 1,3-Dioxolane, Nitroform, Methylene chloride, Dimethylformamide, Sodium sulfate. Hydrochloric acid. Magnesium sulfate. Nitric acid. Sulfuric acid Sulfuryl chloride. Acetic anhydride. Nitric acid. Sodium bicarbonate. Sodium sulfate Nitric acid. Sulfuric acid, Malonamide Nitric acid. Sulfuric acid, Cyanoacetic acid Sulfuric acid, Acetasalicyclic acid. Potassium nitrate Nitroform, Diethyl ether, 1-Bromo-l-nitroethane, Sodium sulfuate... 

Sulfite paper has a relatively short life span, since residual acid will continue to hydrolyze the cellulose and cause embrittlement. Further sources of acid include aluminum sulfate (which is added together with resin to suppress bleeding or feathering of ink into the paper) and S02 and NO from the atmosphere. Much of the world s library collections and archives will soon be lost as the paper crumbles. Various deacidification treatments (e.g., with ammonia, morpholine, cyclohexylamine carbamate, or diethyl-zinc) have been proposed and tried, but at best they can only halt the process of embrittlement and cannot reverse it.14 With the move to kraft pulping, alkaline peroxide bleaching, and increasing use of precipitated calcium carbonate as a filler, the high quality papers produced today are intrinsically acid free and should also resist subsequent acidification by S02-polluted air fairly well. 

A 1-M hexane solution of di isobutyl aluminum hydride (400 mL, 0.40 mol) (Note 10) is added dropwise with stirring at 0°C oxer a 1-hr period. The solution is stirred for 2 additional hr at 0°C. To quench the reaction 200 mL of methanol is carefully added to the stirred reaction mixture, followed slowly at first then more rapidly with 400 mL of water and then 300 mL of 10 sulfuric acidt solution. After the mixture is stirred for 10 min, it is transferred to a separatory funnel and 500 mL of 10% sulfuric acid solution is added. The separatory funnel is shaken vigorously for 5 min and the organic phase 1s separated. The aqueous phase is extracted four times with 300 mL of diethyl ether. The organic phases are combined and washed twice with 300 mL of saturated sodium bicarbonate solution, twice with 300 mL of water, twice with 300 mL of brine, and dried over magnesium sulfate. Solvent removal on a rotary evaporator followed by short path distillation at reduced pressure affords 31-34 g (40-44%, based on 3-ethoxy-6-methyl-2-cyclohexen-l-one) of 4-(E-l,2-dichlorovinyl )-4-methy 1-2-cyclohexen-l-one (1) as a colorless oil, bp 75-78°C (0.1 mm) (Note 11). 

To a solution of 2-[o-t-butyl-a-phenylbenzyl)oxy]-N,N-dimethyl acetamide in anhydrous diethyl ether is added portionwise with stirring and while refiuxing lithium aluminum hydride. After the addition is completed, refluxing is continued overnight. The reaction mixture still contains some lithium aluminum hydride which is decomposed by the addition of water. The mixture is filtered, the ethereal solution separated and dried over sodium sulfate. Diethyl ether is removed from the ethereal solution by distillation. There is obtained 2-[(o-t-butyl-a-phenylbenzyl)oxy]-N,N-dimethylethylamine. 

Phenyl 4-(Phenyltelluro)phenyl Tellurium2 A 500-ml, three-necked, round-bottom flask is fitted with a cold-finger condenser charged with dry ice/ethanol, a nitrogen inlet, and a magnetic stirrer. 250 ml of liquid ammonia are condensed into the flask, 1.6 g (4 mmol) of diphenyl ditellurium and then pieces of sodium are added until the blue color persists. A very small amount of diphenyl ditellurium is added to discharge the blue color followed by 1.13 g (4 mmol) of 4-bromoiodobenzene, and the mixture is irradiated for 220 min. The reaction is quenched by addition of 10 ml of distilled water, the ammonia is allowed to evaporate, the residue is diluted with 100 ml of water, and the whole is extracted three times with 100 ml of diethyl ether. The extract is dried with anhydrous sodium sulfate, the solvent is distilled off, and the residue is chromatographed on neutral aluminum oxide with petroleum ether as eluent yield 0.58 g (30%) m.p. 88-907... 

Methoxy-2-phenyl-l-benzotellurinium Perchlorate1 1.81 g (5.0 mmol) of 7-methoxy-2-phenyl-4-oxo-4H-1 -benzotellurin are dissolved in 20 ml] of dry tetrahydrofuran, the solution is cooled to — 78°, and 5.5 ml] of a 20% solution of diisobutyl aluminum hydride in hexane are added dropwise via a syringe. The resultant mixture is then slowly warmed to 20°, 20 m/] of a 1.0 molar sodium hydroxide solution are added, the mixture is stirred at 20° for 1 h, and is then poured into 100 ml] of diethyl ether. The organic phase is washed with brine, dried with anhydrous sodium sulfate, filtered, and concentrated. The residue is dissolved in 25 ml] of acetic acid, 2 ml] of 70% perchloric acid are added, and the solution is allowed to cool. The resultant red precipitate is filtered off, washed with several portions of diethyl ether, and air-dried yield 1.13 g (50%) m.p. 150° (dec). 

MethylphenyI)-teUuraxanthene1 0.5 g (13 mmol) of lithium aluminum hydride and 3.0 g (23 mmol) of aluminum trichloride are suspended in 50 ml of absolute diethyl ether. To the stirred suspension at 20 are added 1.60g (4 mmol) of 9-hydroxy-9-(4-methylphenyl)-telluraxanthene and the mixture is heated under reflux for 1 h. After cooling, it is diluted by slow addition of 50 ml of diethyl ether, the resultant solution is poured into 100 ml of 20% aqueous sulfuric acid, the mixture is filtered, and the filtrate separated into two layers. The aqueous layer is washed with two 50 ml portions of diethyl ether. The organic phases are combined, dried with anhydrous sodium sulfate, filtered, and the filtrate is evaporated yield 1.23 g (80%) m.p. 1G3°. 

Hydroxytelluraxanthene 1.5 g(39 mmol) of lithium aluminum hydride is suspended in 100 ml of absolute diethyl ether, 9.24 g (30 mmol) of thoroughly ground teiluraxanthone are added in small portions to the stirred suspension kept at 20°, and the resultant mixture is stirred for 2 h. 100 ml of ethyl acetate are then added to the cooled, vigorously stirred reaction mixture, followed by a saturated aqueous ammonium chloride solution. The hydrolyzed mixture is filtered, the organic layer is separated, the aqueous phase is extracted twice with diethyl ether, and the organic solutions are combined, washed with water, dried with anhydrous sodium sulfate, filtered, and evaporated. The residue is chromatographed on aluminum oxide with benzene as the mobile phase yield 7.2 g (77%) m.p. 110 112°. 

Cyclization of 1,3-diiodides takes place smoothly. 1-Benzyl-1-methylcyclopropane was obtained in 97% yield from 2,2-bis(iodomethyl)-l-phenylpropane on treatment with lithium aluminum hydride in diethyl ether, in 100% yield with chromium(II) sulfate in dimethylformamide/ water, and in 94% yield with tributyltin hydride in benzene. 3,3-Bis(iodomethyl)pentane gave 1,1-diethylcyclopropane on treatment with diethyl ether in 93% yield. ... 

Reducing agents Aluminum hydride. Bis-3-methyl-2-butylborane. n-Butyllithium-Pyridine. Calcium borohydride. Chloroiridic acid. Chromous acetate. Chromous chloride. Chromous sulfate. Copper chromite. Diborane. Diborane-Boron trifluoride. Diborane-Sodium borohydride. Diethyl phosphonate. Diimide. Diisobutylaluminum hydride. Dimethyl sulfide. Hexamethylphosphorous triamide. Iridium tetrachloride. Lead. Lithium alkyla-mines. Lithium aluminum hydride. Lithium aluminum hydride-Aluminum chloride. Lithium-Ammonia. Lithium diisobutylmethylaluminum hydride. Lithium-Diphenyl. Lithium ethylenediamine. Lithium-Hexamethylphosphoric triamide. Lithium hydride. Lithium triethoxyaluminum hydride. Lithium tri-/-butoxyaluminum hydride. Nickel-aluminum alloy. Pyridine-n-Butyllithium. Sodium amalgam. Sodium-Ammonia. Sodium borohydride. Sodium borohydride-BFs, see DDQ. Sodium dihydrobis-(2-methoxyethoxy) aluminate. Sodium hydrosulflte. Sodium telluride. Stannous chloride. Tin-HBr. Tri-n-butyltin hydride. Trimethyl phosphite, see Dinitrogen tetroxide. 

A double metal oxide sulfate solid superacid (alumina-zirconia/ persulfate, SA-SZ) can be prepared by treatment of a mixture of aluminum hydroxide and zirconium(IV) hydroxide with an aqueous solution of ammonium persulfate, followed by calcination at 650°C. This catalyst can be efficiently utilized in the benzoylation of arenes with benzoyl and parfl-nitrobenzoyl chloride (Table 4.22), giving BPs in interesting yields. Even if 1 g of catalyst is needed for 40 mmol of chloride, the process seems to be quite useful because the catalyst can be readily regenerated by heating after washing with acetone and diethyl ether and reused four times. 

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