Aluminum potassium tartrate

In many cases separation of the aluminum salts and cyclohexanone cannot be carried out as in the above experiment. In these cases the aluminum salts can generally be removed by washing with dilute hydrochloric acid or with aqueous Rochelle salt (sodium potassium tartrate) solution. Cyclohexanone and cyclohexanol can be conveniently removed by steam distillation as described in the following experiment. 

D. Tris[(2-peiiluorohexyl)ethyl]tin hydride (Note 7). A 1-L, three-necked flask and a stirring bar are dried in an oven. The fluorous tin bromide (13.8 g, 11.1 mmol) is dissolved in dry ether (275 mL) and transferred to the dried three-necked flask equipped with a thermometer, stirring bar, and an outlet to argon. The solution is cooled to O C. AIM solution of iithium aluminum hydride (LAH) in ether (11.1 mL, 11.1 mmol) is added dropwise over 45 min to the solution. The addition rate is adjusted to maintain a temperature between 0° and 1°C. The reaction mixture is stirred for 6 hr at 0°C. Water (75 mL) is slowly added (initially dropwise) with stirring to the ice-cold mixture. Sodium potassium tartrate (20%) (250 mL) is added and the mixture is transferred to a 1-L separatory funnel. The ethereal layer is separated and the aqueous layer is extracted three times with ether (3 x 100 mL). The combined extracts are dried with magnesium sulfate and vacuum filtered into a 1-L, round-bottomed flask. The solvent is evaporated under reduced pressure. The cmde product is distilled under a reduced pressure of 0.02 mm at 133-140°C to provide 11.3 g (9.69 mmol, 87%) of the pure product as an oil (Notes 8 and 9). 

To a cooled (0°C) solution of 2 [178 mg, 0.5 mmol (from two runs)] in dry THF (10 mL), lithium aluminum hydride (20 mg, 0.5 mmol) was added. The cooling bath was removed and the mixture was allowed to attain room temperature. After 30 min the solution was poured into 20 mL of saturated solution of sodium potassium tartrate, and the two-phase mixture was stirred at room temperature. After 1.5 h the mixture was extracted with ether (3 X 20 mL) and the combined organic extracts were washed with water (20 mL) and brine, dried (MgS04), and concentrated under reduced pressure at low temperature (cold-water bath) to avoid losses of the volatile 6-hydroxymethyl-2-methoxy-5,6-dihydro-2H-pyran. 

To a clean dry test tube at the desired temperature, calculated amounts of methyl chloride, 2,4,4-trimethyl-1 -pentene, n-nonane and the alkylaluminum compound were added and the test tube was stoppered with a rubber septum cap. The content of the test tube was mixed by shaking and the calculated amount of f-butyl chloride in methyl chloride solvent was rapidly added with a syringe. After 25 min the reaction was terminated by slow addition of prechilled methanol. During termination the septum cap was removed to prevent pressure build-up due to the formation of gaseous products. The tube was removed from the drybox and the solvent was slowly evaporated. To facilitate the separation of the organic products from the aluminum oxide residues a saturated aqueous sodium-potassium tartrate solution was slowly added at 0° C. On adding excess water, the aluminum oxide-tartrate complex can be dissolved to yield well separated aqueous and organic layers. The... 

The problem is apparently due to some residual aluminum that is hard to remove. If, however, the reduction is carried out in a iV-methylmorpholine solution, followed by addition of potassium tartrate, a pure product can be isolated. A -Methylmorpholine is a good solvent for reductions of various macromolecules with metal hydrides.In addition, the solvent permits the use of strong NaOH solutions to hydrolyze the addition complexes that form. Other polymers that can be reduced in it are those bearing nitrile, amide, imide, lactam, and oxime pendant groups. Reduction of polymethacrylonitrile, however, yields a product with only 70% of primary amine groups. Complete reductions of pendant carbonyl groups with LiAlH4 in solvents other than A -methyl-morpholine, however, were reported. Thus, a copolymer of methyl vinyl ketone with styrene was fully reduced in tetrahydrofuran. ... 

Aluminum nitrate Aluminum nitrate nonahydrate Ammonium carbonate Ammonium fluoride Antimony potassium tartrate... 

Ether containing LiAlH4 added to a soln. of AIGI3 in anhydrous ether followed immediately by an ethereal soln. of frans-2,3-diphenylacrylic acid, refluxed 1 hr., then hydrolyzed by dropwise addition at 0° of aq. 20%-sodium potassium tartrate trans-2,3-diphenylallyl alcohol. Y 72%.—The presence of AIGI3, which produces a mixture rich in aluminum hydride, improves the yield. J.H. Brewster and H. O. Bayer, J. Org. Ghem. 29, 105 (1964). 

Table 6 Hsts the leavening acids and the corresponding rates of reaction. The leavening acids most frequently used iaclude potassium acid tartrate, sodium aluminum sulfate, 5-gluconolactone, and ortho- and pyrophosphates. The phosphates iaclude calcium phosphate [7758-23-8] CaHPO, sodium aluminum phosphate, and sodium acid pyrophosphate (66).

DOUBLE SALT. A hydrated compound resulting from crystallization ol a mixture of ions in aqueous solution. Common examples arc the alums, made by ciystallizing from solution either potassium or ammonium sulfate and aluminum sulfate Rochelle salt (potassium sodium tartrate), made from a water solution of potassium acid tartrate treated with sodium carbonate and Mohr s salt (fertous ammonium sulfate), crystallized Iruin mixed solutions of ferrous sulfate and ammonium sulfate. 

Codeine sulfate trihydrate Ammonium hydroxide Aluminum isopropoxide Potassium sodium tartrate tetrahydrate Palladium on carbon... 

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