Amine sulfate

In the first case (22), almost stoichiometric amounts of sulfuric acid or chlorosulfonic acid are used. The amine sulfate or the amine chlorosulfate is, first, formed and heated to about 180 or 130°C, respectively, to rearrange the salt. The introduction of the sulfonic acid group occurs only in the ortho position, and an almost quantitative amount of l-aminoanthraquinone-2-sulfonic acid is obtained. On the other hand, the use of oleum (23) requires a large excess of SO to complete the reaction, and inevitably produces over-sulfonated compound such as l-amino-anthraquinone-2,4-disulfonic acid. Addition of sodium sulfate reduces the byproduct to a certain extent. Improved processes have been proposed to make the isolation of the intermediate (19) uimecessary (24,25). 

C20H25NO4 73074-37-2) see Atracurium besilate (/t)-tetrabydropapaverine 7V-acetyl-L-leucinate (C2gH4(,N207 141109-12-8) see Cisatracurium besylate ( )-tetrabydropapaverine bydrocbloride (C20H26CINO4 6429-04-5) see Cisatracurium besylate [ -( , 5 )]-2,3,4,9-tetrabydro-7V-(l-phenylethyt)-lff-carbazol-3-amine sulfate (1 1)... 

Figure 5.22 Flowsheet for the production of nuclear pure Zr02 by amine-sulfate route.

In a 2-1. beaker is placed 75 g. (0.4 mole) of 3-bromo-4-amino-toluene (Note 1), and to it is added the hot diluted acid obtained by adding 72 cc. of concentrated sulfuric acid to 200 cc. of water. The clear solution is stirred and cooled to about 15°, after which 180 g. of ice is added the amine sulfate usually separates. As soon as the temperature has dropped below +5°, a solution of 32.2 g. (0.47 mole) of sodium nitrite in 88 cc. of water is added from a dropping funnel, the stem of which extends below the surface of the liquid. The temperature of the solution is kept below +5° during the addition, which requires about fifteen minutes. The solution is stirred for five minutes after the addition of all the sodium nitrite, and 300 g. of cold water, 3 g. of urea, and 300 g. of cracked ice are then added successively. The solution is kept in an ice bath until used. 

As noted earlier (see section 12.3.1), the Amex process, which uses long-chain amines, is preferred over the Dapex process, which uses HDEHP, for solvent extraction of uranium from H2SO4 leach solutions. Because the surfactant properties of amine sulfates are conducive to formation of objectionable emulsions, the Amex process is very sensitive to the presence of solids in the H2SO4 leachate. For acceptable phase coalescence in the Amex process, feeds should contain no more than 20 ppm solids. The Dapex process can tolerate feeds containing as much as 100 ppm solids. 

An additional mole of ammonium sulfate per mole of final lactam is generated during the manufacture of hydroxyl amine sulfate [10039-54-0] via the Raschig process, which converts ammonia, air, water, carbon dioxide, and sulfur dioxide to the hydroxylamine salt. Thus, a minimum of two moles of ammonium sulfate is produced per mole of lactam, but commercial processes can approach twice that amount. The DSM/Stamicarbon HPO process, which uses hydroxylamine phosphate [19098-16-9] in a recycled phosphate buffer, can reduce the amount to less than two moles per mole of lactam. Ammonium sulfate is sold as a fertilizer. However, because H2S04 is released and acidifies the soil as the salt decomposes, it is alow grade fertilizer, and contributes only marginally to the economics of the process (145,146) (see Caprolactam). 

Catalytic cyclodehydrogenation of 5-amino-2-ethylthiophenol affords 6-aminobenzo[6]thiophene.239,241 6-Acetamido-2,3-di-bromo-,77 6-acetamido-2-bromo-3-methyl-,102 6-acetamido-3-bromo-2-methyl-,102 and 6-acetamido-3-bromobenzo[f>]thiophene107 may be obtained from the corresponding 6-acetyl compound by means of the Schmidt reaction. In some cases the 6-acetamido compound is accompanied by a smaller amount of the amine sulfate.102,107 6-Aminobenzo[6]thiophene may be converted into 6-chloro- or 6-cyanobenzo[6]thiophene by means of the Sandmeyer reaction.241... 

The extraction of uranium(VI) from sulfate media by amine sulfates of different types lies in the order tertiary > secondary > primary, whereas the extraction of iron(III) lies in the reverse order,195 206 with the result that tertiary amines are the obvious choice for the selective extraction of uranium in the presence of iron. 

Hygroscopicity and caking of AN and its mixts with Amin sulfate) 48)W. Kretzschmar, ZAnorgChem 219,17-34(1934) CA 28,7191(l934)(Thermal decompn of AN) 49)H,Tram H.Welde, AngChem 47,782-3... 

Khier et al. [30] determined mefenamic acid after complexation with copper(II) amine sulfate. The complex is extracted with chloroform and treated with diethyldithiocarbamate solution, whereupon another copper (II) complex (wavelength maximum of 430 nm) is formed. Beer s law is followed over the mefenamic acid concentration range of 6 18 pg/mL. The method was applied successfully to the determination of mefenamic acid in bulk samples and in pharmaceutical preparations, with recoveries of 98.0-101.0%. 

Alpdogan and Sungur [50] developed an indirect atomic absorption spectroscopy method for the determination of mefenamic and flufenamic acids, and diclofenac sodium, based on the complexation with copper (II) amine sulfate. The complex was extracted into chloroform, and the concentrations of substances were determined indirectly by AAS measurement of copper after re-extraction into 0.3 N nitric acid solution. The developed method was applied to the assay of the substances in commercial tablet formulations. The results were statistically compared with those obtained by HPLC method by t- and F tests at 95% confidence level. Calculated t and F values were both lower than the table values. 

Smith (52,53) has investigated the affect of various additives on the rate constants for the hydrogenation of terpenes. The most effective additive tried was palmitic acid. Soaps, amines, sulfated alcohols, quaternary ammonium salts, and amides also increased the rate. 

DIAMINOTOLUENE SULPHATE 2-METHYL-I.4-BENZENEDIAMINE SULFATE 2-METHYL-p-PHENYXENEDIAMINE SULPHATE NCI-C01832 p-TOLUENEDIAMINE SULFATE 2,5-TOLUENEDI-AMINE SULFATE TOLUENE-2.5-DIAMINE, SULFATE (1 1) (SCI) p-TOLUENEDIAMINE SULPHATE TOLUENE-2,5-DIAMINE SULPHATE p-TOLUYLENE-DIAxMINE SULPHATE TOLUYLENE-2.5-DIAMINE SULPHATE p-TOLYLENEDIAMINE SULPHATE... 

A solution of 20 g. (0.165 mole) of m-xylidine in 200 g. of concentrated sulfuric acid is cooled to 5°, and 16.5 g. of concentrated nitric acid is added slowly with stirring. During this operation and for an additional 30-minute stirring period, the temperature of the reaction mixture is held below 15°. Pouring the mixture on crushed ice precipitates the amine sulfate, which is separated by filtration. The solid is treated with 10% aqueous sodium carbonate solution, and the resulting free amine is recrystallized from a 50% aqueous ethanol solution. The yield of 2,4-dimethyl-5-nitroaniline is 23 g. (84%), and the product melts at 123-124°. 

Alcohols, phenols, hydroxylamines, and amines can be sulfated, as can endogenous substrates such as steroids, polysaccharides, and biogenic amines. Sulfation can lead to metabolites that are more toxic than their precursors (Fig. 6). 

N-Methyl-N-methoxycarbamoyl chloride made by phos-genation of methoxy methyl amine hydrochloride is a very useful intermediate for the synthesis of N-methoxy ureas herbicides. However, we found the method to be unsatisfactory for the production on a large scale, because of rather low yields and also of technical difficulties. To overcome these problems, we developed a new procedure based on the reaction of phosgene with methoxy methyl amine sulfate as depicted in scheme 124. Sulfuric acid formed is easily removed by decantation (Ref. 177). 

In the sulfonation of aromatic substrates containing a free amino group with hot concentrated sulfuric acid, the initially formed amine sulfate may rearrange to yield the required sulfonic acid. Thus, when aniline (31) is heated with concentrated sulfuric acid at 200°C (the baking process ), the amine sulfate (32) is probably converted into phenylsulfamic acid (33) which subsequently rearranges by migration of the sulfonic acid group into orthanilic acid (34) and finally to the most thermodynamically stable sulfanilic acid (35) (Scheme 18). 

---