Potassium hydroxide perchlorate

Delsonine is amorphous and is isomerised to isodelsonine, m.p. 108-111°, by boiling with potassium hydroxide in alcohol. The following crystalline salts of delsonine were prepared perchlorate, C24H4 0jN. HCIO4, m.p. 216° (dec.), [a] f + 23° (MeOH) hydriodide, B. HI, m.p. 202°. The base contains at least four methoxyl groups. 

ICA 97)19]. Compound 163 (R = Br) and perchloric acid yield 164, where the monodentate pyrazolate ligand is protonated. Potassium hydroxide regenerates 163 (R = Br). Dicationic complexes of the type 164 can alternatively be produced from [Rh2(r/ -Cp )2(/x-0H)3]Cl04 and perchloric acid in the presence of excess pyrazole, 4-bromopyrazole, 3-methylpyrazole, or 3,5-dimethylpyrazole. 

This was reacted with chlorine to give the dichloropregnene compound, then with selenium dioxide to give the dichloropregnadiene compound. By hydrolysis with methanolic potassium hydroxide there was obtained the free 6a-fluoro-9a,11/3-dichloro-A -pregnadiene-16a,-17a,21-triol-3,20-dione. By treatment with acetone in the presence of perchloric acid, the 16,17-acetonide of 6a-fluoro-9a,11/3-dichloro-A -pregnadiene 16a,17a,21-triol-3,20-dione was formed. 

Amino-3,5-dimethylisoxazole (372, R = H) gave an iV-tosyl derivative (372, R = tosyl), which by treatment with methyl fluorosulfonate followed by perchloric acid gave the salt 371, R = R = R = Me, R = tosyl, X = C104. Attempts to isolate the meso-ionic sul-fonamidate (370, R = R = R = Me, R = tosyl) by treatment of the salt with potassium hydroxide or triethylamine were unsuccessful, but spectroscopic evidence for its formation in solution has been offered. 

It will be observed that potassium hypochlorite is the first product of the action of chlorine upon potassium hydroxide, and the hypochlorite is successively converted into the chlorate or perchlorate, before it is finally all transformed into the chloride. The hypochlorite, chlorate, and perchlorate thus represent intermediate stages in the reaction 4K0H+2C12... 

M solutions of 6HQ (Kodak) in distilled, deionized water containing distilled perchloric acid (Aldrich 99.999%) or potassium hydroxide pellets (Aldrich 99.99%) were circulating in a flow cell (2.5 mm optical path length). The subpicosecond transient absorption experiment has been already described [5]. The polarizations of the laser pump (266 nm) and continuum probe pulses were set at the magic angle (overall time resolution 300 fs). 

Oxidation of 2-(3-aminopropyl-l,2,3,4-tetrahydroisoquinoline with mercuric acetate in 4% aqueous acetic acid at 50°C for 6 h, and then at room temperature overnight followed by the treatment of the filtered solution with 20% potassium hydroxide solution, yielded 1,3,4,6,7,llb-hexahydro-2//-pyrimido[2,l-a]isoquinoline (16, R = R1 = H) in 27% yield (73JOC437). 1,3,4,6,7,llb-Hexahydro-2//-primido[2,l-a]isoquinolines (16, R = H, MeO, R1 = H) and their 2-oxo derivatives (18, R = H, MeO, R1 = H) were obtained from 2-(3-aminopropyl)- and 2-(2-aminocarbonylethyl)-3,4-dihydroisoquinolinium salts (17 and 19, R = H, MeO, R1 = H) by treatment with a base (62CB2122,62MI1). The adjustment of the pH value of a solution of l-methyl-2-(2-aminocarbonylethyl)-3,4-dihydroisoquinolinium perchlorate (19, R = H, R1 = Me, X = C104) in 10% aqueous acetic acid with sodium carbonate to 9 yielded 1 lb-methyl-1,3,4,6,7,1 lb-hexahydro-2//-primido[2,l-a]isoquinolin-2-one (111) (93KGS499). 

H. Stamm also measured the solubilities of the salts of the alkalies in liquid ammonia —potassium hydroxide, nitrate, sulphate, chromate, oxalate, perchlorate, persulphate, chloride, bromide, iodide, carbonate, and chlorate rubidium chloride, bromide, and sulphate esesium chloride, iodide, carbonate, and sulphate lithium chloride and sulphate sodium phosphate, phosphite, hypophosphite, fluoride, chloride, iodide, bromate, perchlorate, periodate, hyponitrire, nitrite, nitrate, azide, dithionate, chromate, carbonate, oxalate, benzoate, phtnalate, isophthalate ammonium, chloride, chlorate, bromide, iodide, perchlorate, sulphate, sulphite, chromate, molybdate, nitrate, dithionate, thiosulphate, persulphate, thiocyanate, phosphate, phosphite, hypophosphite, arsenate, arsenite, amidosulphonate, ferrocyanide, carbonate, benzoate, methionate, phenylacetate, picrate, salicylate, phenylpropionate, benzoldisulphonate, benzolsulphonate, phthalate, trimesmate, mellitate, aliphatic dicarboxylates, tartrate, fumarate, and maleinate and phenol. 

The absorption train is composed of a tube packed with water absorbent, a second tube packed with a carbon dioxide absorbent, and a guard tube packed with equal volumes of the water and carbon dioxide absorbents. Anhydrous magnesium perchlorate (MgC104) is commonly used for the water absorbent, while sodium hydroxide (NaOH) or potassium hydroxide (KOH) impregnated in an inert carrier is used as the carbon dioxide absorber. 

A solution of 70% perchloric acid (60 ml) in water (280 ml) was added to a stirred solution of 5a-androst-2-en-17-one (200.0 g) in ether (1.15 I) at 15°C followed by portionwise addition of N-bromacetamide (112.0 g) over 10 min. After stirring for 1 h the precipitated white crystalline solid was filtered off, washed neutral with ether and water and crystallised to give 2p-hydroxy-3a-bromo-5a-androstan-17-one (172.0 g). The ether layer of the filtrate was washed neutral, dried (Na2S04) and concentrated to give a second crop (28.0 g). The two crops (200.0 g) were suspended in methanol (1 L), 10 N aqueous potassium hydroxide solution (100 ml) added and the mixture slowly distilled over 45 min. Addition of water precipitated the product as a white solid which... 

To an ice-cold solution of 35.1 g. (0.1 mol) of tripotassium trimetaphosphimate in 95 ml. of water is added, slowly, 62 ml. of 72% perchloric acid so that the temperature does not exceed 25°. The potassium perchlorate is filtered off and washed with 15 ml. of 5% perchloric acid. The combined filtrates are transferred to a 200-ml. round-bottomed flask and evaporated at reduced pressure. A Dry Ice trap and potassium hydroxide pellets are used before the oil pump. The solution is stirred with a magnetic stirring bar and is heated in a water bath at not over 31°. When nearly but not quite dry, the solids are slurried in ethyl acetate-methanol (80/20 by volume) to remove any crystallized potassium perchlorate, transferred to a Buchner funnel and rinsed, using a total of 125 ml. of the above solvent, then... 

Mobile Phase Transfer 35.1 g of sodium perchlorate, 1.40 g of monobasic potassium phosphate, 7.0 mL of 1 A potassium hydroxide, and 40 mL of methanol to a 1000-mL volumetric flask, dilute to volume with water, and mix. Adjust the pFI to 7.2 with 1 N potassium hydroxide. 

Perform a blank determination (see General Provisions), and make any necessary correction, recording the net volume of perchloric acid consumed as V. Calculate the number of milligrams of potassium hydroxide equivalent to the sodium salts per gram of sample by the formula... 

The presence of the /3-hydroxypropionic ester unit in deacetylpicraline is established by oxidation with chromic acid in acetone, which yields an aldehyde base, picralinal, C21H22N2O4 the latter is readily deform yla ted by short treatment with methanolic potassium hydroxide, which affords picrinine in quantitative yield. Reduction of picralinal with sodium borohydride regenerates deacetylpicraline. Vigorous treatment of deacetylpicraline with sodium borohydride gives a noncrystalline indoline base, which exhibits the UV-absorption of an anilinium ion in concentrated perchloric acid hence, the Na-carbinol-amine ether function must have suffered reduction. Since acetylation of the noncrystalline base gives a product which exhibits acylaniline UV-absorption, picraline and its derivatives must contain an NaH group (53, 54). 

Other substances. The concentrations of acids and bases and alkalis could be listed as follows acetic acid > 25% concentration, hydrochloric acid > 25% concentration, nitric acid > 20% concentration, chromic acid, hydrofluoric acid, perchloric acid > 10% concentration, sulfuric acid > 15% concentration, fuming sulfuric acid, ammonium hydroxide > 35% by weight of gas, potassium hydroxide (caustic potash), sodium hydroxide > 5% concentration, aluminum chloride, bromine, phosphorous trichloride, potassium bifluoride, sodium hypochlorite > 10% concentration, and zinc chloride. 

The perchloric acid extraction procedure described by Kraus and Rein-both (K27) involves a perchloric acid extraction followed by neutralization with a potassium hydroxide solution. Riss et al. (R3) reported recoveries ranging from 68 to 87% for the adenosine-, cytidine-, guanosine-, and uridlne-5 -nucleotides, with a mean recovery of 78%. Other investigators have used the PCA extraction procedure in the analysis of nucleotides... 

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