Sodium preparation, alternative

Calcium hypochlorite may be prepared by passing chlorine into a slurry of lime and sodium hydroxide. Alternatively, chlorine is passed into a solution of hydrated lime to produce bleaching powder, CaCl(0Cl) H20 ... 

Synthesis (Krauli (E. Merck), 1925, Juby et al., 1968, Ehrhart and Ruschig 1972) Thebaine is oxidized with hydrogene peroxide to 14-hydroxycodeinone (Bentley 1954, Hauser 1974), which is hydrogenated directly or via its oxime, or its bromination products to oxycodone. The reduction of 14-hydroxycodeinone can also be carried out with sodium hydrosulfite. Alternatively 14-hydroxycodeinone is prepared by oxidation of codeine. 

Dissolve the appropriate methyl ester in methanol, and saponify as previously described for preparation of retinol from retinyl acetate After saponification, add water, and then acidify with dilute glacial-acetic acid make sure the solution is acidic to litmus paper. (In aqueous-alkaline solution, retinoid carboxylic acids remain as sodium salts, and are not extracted by organic solvents.) Extract the retinoid-carboxylic acid with diethyl ether two or three times (Note that hexane is not a good solvent for these polar retinoids.) Then wash the ether extract with water, and dry it over anhydrous sodium sulfate. Alternatively, if the volume is small, vortex and centrifuge the sample, remove any water, and evaporate the solvent The retinoid-carboxylic acids usually are obtained as yellow solids. Do not add any (not even a trace) HCl to 5,6-epoxy retinoids, because they instantaneously undergo isomerization to 5,8-epoxy retinoids, this change in structure is readily confirmed by the change m absorption spectrum (Table 1). 

Deshmukh et al. demonstrated that triphosgene can also be used to prepare dialkylcar-bamoyl azides from tertiary amines and sodium azide. Alternatively, acyl azides (e.g. 303) can be converted via a one-step procedure from carboxylic acids using bis(2-methoxyethyl)aminosulfur trifluoride (Deoxo-Fluor) (Scheme 3.46). ... 

After completing a production run the mold surfaces should be washed scrupulously with a mild alkaline solution such as sodium nitrate. Alternatively dissolve 1 kilo (2.21bs) of soda crystals in 1 liter (2.11 U.S. pints) of water. Use the prepared solution to wash the mold surfaces. After drying, the mold surfaces should be sprayed with an oil or silicone base spray. 

Refractionation of the low-boiling impurities gives a further quantity of the acetoacetate, but if the initial distillation has been carefully conducted, the amount recovered is less than i g., and the refractionation is not worth while. If possible, complete the preparation in one day. If this is not possible, it is best to allow the cold crude sodium derivative (before acidification) to stand overnight, the flask being closed by a cork carrying a calcium chloride tube the yield will now fall to about 38 g. Alternatively, the crude ester may be allowed to remain overnight in contact with the sodium sulphate, but in this case the yield will fall to about 30 g. 

Alternatively, prepare the sodium meta-arsenite solution by dissolving 39 6 g. A.R. arsenious oxide and 32 g. of A.R. sodium hydroxide in 600 ml. of water. 

I) An alternative procedure is to cool the solution containing the sodium sul. phanilate and sodium nitrite in a bath of crushed ice to about 5° and then add 10-5 ml. of concentrated hydrochloric acid diluted with an equal volume of water slowly and with stirring the temperature must not be allowed to rise above 10 and an excess of nitrous acid should be present (the solution is tested after standing for 5 minutes). The subsequent stages in the preparation—addition of dimethyl-aniline solution, etc.—are as above. 

A useful alternative to catalytic partial hydrogenation for converting alkynes to alkenes IS reduction by a Group I metal (lithium sodium or potassium) m liquid ammonia The unique feature of metal-ammonia reduction is that it converts alkynes to trans alkenes whereas catalytic hydrogenation yields cis alkenes Thus from the same alkyne one can prepare either a cis or a trans alkene by choosing the appropriate reaction conditions... 

Both reactants m the Williamson ether synthesis usually originate m alcohol pre cursors Sodium and potassium alkoxides are prepared by reaction of an alcohol with the appropriate metal and alkyl halides are most commonly made from alcohols by reaction with a hydrogen halide (Section 4 7) thionyl chloride (Section 4 13) or phosphorus tri bromide (Section 4 13) Alternatively alkyl p toluenesulfonates may be used m place of alkyl halides alkyl p toluenesulfonates are also prepared from alcohols as their imme diate precursors (Section 8 14)... 

Plutonium Purification. The aqueous feed for the second plutonium cycle is typically prepared by adding HNO and an excess of sodium nitrite, NaN02, to destroy the excess reductant and oxidize the Pu to the more extractable Pu . An alternative approach which reduces the amount of salt in the Hquid waste involves absorbing nitrogen tetroxide, N2O4, as a substitute for the NaN02 ... 

Aluminum acetylsaHcylate is a tasteless, nonbasic, stable, alternative therapeutic salt to aspirin (83). Also called aluminum aspirin, it is an insoluble white to off-white powder prepared by reaction of aluminum isopropoxide with sodium acetylsaHcylate in an organic solvent. The product precipitates from the reaction mixture (83). Standards requke that aluminum aspirin contain not less than the equivalent of 80% aspirin, corresponding to 90% purity on an anhydrous basis. The aluminum oxide assay must be 12—17% (81). 

Sulfamation is the formation (245) of a nitrogen sulfur(VI) bond by the reaction of an amine and sulfur trioxide, or one of the many adduct forms of SO. Heating an amine with sulfamic acid is an alternative method. A practical example of sulfamation is the artificial sweetener sodium cyclohexylsulfamate [139-05-9] produced from the reaction of cyclohexylamine and sulfur trioxide (246,247) (see Sweeteners). Sulfamic acid is prepared from urea and oleum (248). Whereas sulfamation is not gready used commercially, sulfamic acid has various appHcations (see SuLFAMiC ACID AND SULFAMATES) (249—253). 

Calcium thiosulfate has been prepared from calcium sulfite and sulfur at 30—40°C, or from boiling lime and sulfur in the presence of sulfur dioxide until a colorless solution is obtained. Alternatively, a concentrated solution of sodium thiosulfate is treated with calcium chloride the crystalline sodium chloride is removed at low temperature. Concentrated solutions of calcium thiosulfate are prepared from ammonium thiosulfate and lime the Hberated ammonium ion is recycled to the ammonium thiosulfate process (85). 

Fluoroall l-SubstitutedTitanates. Tetraliexafluoroisopropyl titanate [21416-30-8] can be prepared by the reaction of TiCl and hexafluoroisopropyl alcohol [920-66-17, in a process similar to that used for TYZOR TPT (7). Alternatively, it can be prepared by the reaction of sodium hexafluoroisopropoxide and TiCl ia excess hexafluoroisopropyl alcohol (8). The fluoroalkyl material is much more volatile than its hydrocarbon counterpart, TYZOR TPT, and is used to deposit titanium on surfaces by chemical vapor-phase deposition (CVD). 

Whereas these preparations do not possess the high bacteriostatic activity of quaternary ammonium germicides, they have the alternate advantage of being rapidly functional in acid solution. In comparative experiments of several different disinfectants, the acid—anionic killed bacteria at lower concentration than five other disinfectants. Only sodium hypochlorite and an iodine product were effective at higher dilution than the acid—anionic. By the AO AC use dilution test, the acid—anionic killed Pseudomonas aeruginosa at 225 ppm. Salmonella choleraesuis at 175 ppm, and Staphylococcus aureus at 325 ppm (172). 

Chloroanthraquinone [82-44-0] (41) is an intermediate for manufacturing vat dyes such as Cl Vat Brown 1. 1-Chloroanthraquinone is prepared by chlorination of anthraquinone-l-sulfonic acid with sodium chlorate in hydrochloric acid at elevated temperature (61). An alternative route from 1-nitroanthraquinone (18) using elemental chlorine at high temperature has been reported (62). 

Cl Vat Blue 4 is prepared from 2-arniaoaiitliraquiQoiie (66) by potash fusion in the presence of an oxidising agent such as sodium nitrite or air. An alternative method by dimerization of 1-aminoanthraquinone (17) by using such solvents as dimethyl sulfoxide or tetramethylurea has been reported, and improved methods for this reaction have been cited (135—138). These methods are considered to be advantageous in terms of the yield as well as the availability of starting compounds. 

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