Potassium permanganate, preparation reduction

The reaction mixture is filtered. The soHds containing K MnO are leached, filtered, and the filtrate composition adjusted for electrolysis. The soHds are gangue. The Cams Chemical Co. electrolyzes a solution containing 120—150 g/L KOH and 50—60 g/L K MnO. The cells are bipolar (68). The anode side is monel and the cathode mild steel. The cathode consists of small protmsions from the bipolar unit. The base of the cathode is coated with a corrosion-resistant plastic such that the ratio of active cathode area to anode area is about 1 to 140. Cells operate at 1.2—1.4 kA. Anode and cathode current densities are about 85—100 A/m and 13—15 kA/m, respectively. The small cathode areas and large anode areas are used to minimize the reduction of permanganate at the cathode (69). Potassium permanganate is continuously crystallized from cell Hquors. The caustic mother Hquors are evaporated and returned to the cell feed preparation system. 

Butyroin has been prepared by reductive condensation of ethyl butyrate with sodium in xylene, or with sodium in the presence of chloro-trimethylsilane. and by reduction of 4,5-octanedlone with sodium l-benzyl-3-carbamoyl-l,4-dihydropyridine-4-sulfinate in the presence of magnesium chloride or with thiophenol in the presence of iron polyphthalocyanine as electron transfer agent.This acyloin has also been obtained by oxidation of (E)-4-octene with potassium permanganate and by reaction of... 

This method is widely applicable to the unambiguous synthesis of quinoxalin-2-ones." It involves the intermediate preparation of a l,2,3,4-tetrahydro-2-oxoquinoxaline by the reductive ring closure of the o-nitrophenyl derivative of an a-aminoacid. These derivatives are formed readily from the aminoacid and an o-nitrohalogenobenzene. The final step of oxidation of the tetrahydro- to the dihydro-quinoxa-line is carried out with potassium permanganate or hydrogen peroxide. The preparation of 7-nitroquinoxalin-2-one illustrates the application of this synthesis ... 

Mesitaldehyde may be prepared from mesitylmagnesium bromide by the reaction with orthoformate esters3 or ethoxy-methyleneaniline 3 from acetylmesitylene by oxidation with potassium permanganate,4 from mesitoyl chloride by reduction,5 from mesityllithium by the reaction with iron pentacarbonyl and from mesitylene by treatment with formyl fluoride and boron trifluoride,7 by treatment with carbon monoxide, hydrogen chloride, and aluminum chloride,8 or by various applications of the Gatterman synthesis.9-11... 

Thenoic acid has been prepared in low yield by oxidation of 3-methylthiophene with potassium permanganate,2-4 dilute nitric acid, chromic acid, and hydrogen peroxide,4 and by reductive dechlorination of chloro-3-thenoic acid.4 Starting with 3-iodothiophene, which is difficult to obtain, good yields are obtained by the Grignard procedure 6 or with cuprous cyanide and potassium cyanide in a sealed tube.6... 

Azoxybenzene has been prepared by reduction of nitrobenzene with alcoholic potassium hydroxide,1 with sodium amalgam,2 with hydrogen in the presence of lead oxide,3 with methyl alcohol and sodium hydroxide,4 with sodium methylate and methyl alcohol,5 and by electrolytic reduction 6 by oxidation of azobenzene with chromic anhydride 7 by treatment of /9-phenylhydroxylamine with alkaline potassium permanganate,8 with nitrobenzene,9 with mineral adds,10 and with mercury acetamide,11 and by oxidation of aniline with hydrogen peroxide,12 and with acid permanganate solution in the presence of formaldehyde.13 The procedure described above is a slight modification of one described in the literature.14... 

Adipic acid has been prepared by the following methods the action of silver1 or copper 2 on /3-iodopropionic acid the reduction of mucic add with phosphorus and iodine 3 the electrolysis of the potassium or sodium salts of monoethyl succinate 4 the condensation of ethylene chloride or bromide with malonic ester or cyanoacetic ester and subsequent hydrolysis 5 the oxidation of certain fractions of Baku petroleum 6 the oxidation of cyclohexanol or cyclohexanone with nitric acid 7 or potassium permanganate.8... 

Since many aliphatic primary amines are usually prepared by methods not involving the reduction of a nitroalkane (cf. aromatic amines), their oxidation may provide a useful route to this class of compound. For amines which lead to tertiary nitroalkanes, potassium permanganate appears to be the most satisfactory reagent198 (the preparation of 2-nitro-2-methylpropane, Expt 5.191). In the case of amines which lead to primary or secondary nitroalkanes the oxidant of choice is m-chloroperbenzoic acid, and Expt 5.191 includes a general procedure for this reaction.199... 

Method. Transfer 5 ml of the urine sample into a 35-ml stoppered tube, add 1 ml of hydrochloric acid, mix, and allow to cool add 10 ml of a 5% solution of potassium permanganate, mix, stopper loosely, and allow to stand overnight. Remove the excess potassium permanganate by adding, dropwise. Hydrogen Peroxide Solution (50 volume). Transfer 0.5 ml of the Stannous Chloride Solution to the reduction vessel, turn on the magnetic stirrer and the argon gas flow, and record the baseline absorbance at 253.7 nm. Add 3 ml of the prepared sample, immediately close the reduction vessel, stir for exactly 2 minutes, and record the absorbance at... 

Reduction method was used to prepare potassium type manganese oxide birnessite K-OL-1. The solution of the mixture of ethanol and potassium hydroxide was added slowly to a beaker containing a solution of potassium permanganate with vigorous... 

J-Oisubstitated SH-indoks. 3,3-Disubstituted 311-indoles (3) can be prepared readily by lithium aluminum hydride [or sodium bis-(2-mcthoxyethoxy)aluminum hydride, 3, 260-261 this volume] reduction of 3,3-disubstituted oxindoles (1), followed by oxidation of the indoline (2) with activated manganese dioxide or potassium permanganate in acetone. 

Preparation of the sulphone, according to Steinkopf (Ber., 1920, 53, 1007) 20 gm. dichloroethyl sulphide, dissolved in 100 ml. of an aqueous solution of acetic acid (i i), are shaken with a saturated aqueous solution of 30 gm. potassium permanganate in presence of 20 ml. dilute sulphuric acid, and then allowed to stand. After reduction of the excess permanganate with sulphur dioxide, crystals of the sulphone separate. 

Barium manganate, prepared from potassium manganate and barium chloride [5JJ] or by the reduction of potassium permanganate with potassium iodide in the presence of barium chloride and sodium hydfoxide [5J2], is used for the quantitative oxidation of benzhydrol to benzophenone. The reaction mixture is refluxed in benzene for 0.5-2 h [SJ5]. The result is comparable with and even better than that of oxidation with manganese dioxide [250, 525]. 

For the synthesis of (69), the enol ether (71) from the indanone (70) was carboxylated with COa-n-butyl-Iithium in THF at —70 C to yield (72). The methyl ester (73) was converted into (75) via the maleic anhydride adduct (74), essentially as described in earlier work. Lithium aluminium hydride reduction followed by oxidation with dicyclohexylcarbodi-imide afforded the aldehyde (76). This was condensed with excess (77) to yield a mixture of the diastereomers (78). Oxidation with chromium trioxide-pyridine in methylene dichloride gave (79), which could be converted into the diketone (80) by treatment with excess benzenesulphonylazide. The diketo-lactam (81) was prepared from (80) as described for the synthesis of the analogous intermediate used in the synthesis of napelline. Reduction of (81) with lithium tri-t butoxyaluminohydride gave the desired dihydroxy-lactam (82). Methylation of (82) with methyl iodide-sodium hydride gave (83). Reduction of this lactam to the amine (84) with lithium aluminium hydride, followed by oxidation with potassium permanganate in acetic acid, gave (69). 

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