Ammonium acetate ethers

The covalent character of mercury compounds and the corresponding abiUty to complex with various organic compounds explains the unusually wide solubihty characteristics. Mercury compounds are soluble in alcohols, ethyl ether, benzene, and other organic solvents. Moreover, small amounts of chemicals such as amines, ammonia (qv), and ammonium acetate can have a profound solubilizing effect (see COORDINATION COMPOUNDS). The solubihty of mercury and a wide variety of mercury salts and complexes in water and aqueous electrolyte solutions has been well outlined (5). 

Alcohol sulfates and alcohol ether sulfates separated by HPLC on a styrene-divinylbenzene copolymer column with 4 1 (v/v) methanol and 0.05 M ammonium acetate aqueous solution as the mobile phase were analyzed by simultaneous inductively coupled argon plasma vacuum emission spectroscopy (IPC), monitoring the 180.7-nm sulfur line as a sulfur-specific detector [294]. This method was applied to the analysis of these surfactants in untreated wastewaters. 

Surface water samples often contain surfactants and their metabolites. After Cis-SPE combined with selective elution [7,9,10] the metabolites, PEG and PPG, were observed in the ether fraction (PPG) or in the combined methanol-water and methanol (PEG) fractions, respectively. They could be ionised in the form of their [M + NH4]+ ions applying ESI-FIA-MS(-I-) in combination with ammonium acetate for ionisation support. ESI-LC-MS(-I-) resulted in an excellent separation of both metabolites, as presented in the total ion current (TIC) trace in Fig. 2.9.6(7) together with selected mass traces of PEG (m/z 300, 344 and 388) and PPG (m/z 442, 500, 558) (Am/z 44 and 58) in Fig. 2.9.6(l)-(6) [36],... 

A good method for the preparation of acetamide is to pass ammonia gas into an ethereal solution of acetic anhydride, evaporate the ether and extract the residual mixture of ammonium acetate and acetamide with benzene in an extraction apparatus (Fig. 25). The salt remains undissolved. Amides can also be prepared by the action of ammonia on acid chlorides and esters. 

Bicyclic pyrimidin-4-ones (1100, R = H, n = 0-3 R = Me, n = 1) were also prepared from the appropriate lactim ether and EMME in the presence of ammonia or ammonium acetate [73JAP(K)34897 75MIP1]. Pyrimido[l,2-a]azepine-3-carboxylates (1100, R = H, Ph n = 2) were prepared in the reaction of 7-aminotetrahydro-2//-azepines (R = H, Ph n = 2) and EMME or in the reaction of O-methylcaprolactim and diethyl aminomethylenemalonate in ethanol [73JAP(K)34897 75MIP1]. 

Two hundred and five grams T1 mole) of a-phenylcinnamoni-trile,2 2250 ml. of methanol, and 750 ml. of ether are placed in a 5-1. round-bottomed flask fitted with a two-necked adapter supporting a 1-1. separatory funnel and reflux condenser. The a-phenylcinnamonitrile is dissolved by gentle heating, and the solution is heated under reflux. A solution of 274 g. (4 moles) of 95% potassium cyanide in 600 ml. of water (which has been preheated to 45°) is added rapidly from the separatory funnel (Note 1). A small amount of potassium cyanide precipitates. The solution is heated under reflux for 1 hour, after which a solution of 154 g. (2 moles) of ammonium acetate in 250 ml. of water is added rapidly from the separatory funnel (Note 2). 

Phenylacetamide has been obtained by a wide variety of reactions from benzyl cyanide with water at 250-260° 6 from benzyl cyanide with water and cadmium oxide at 240° 6 from benzyl cyanide with sulfuric acid 7 8 by saturation of an acetone solution of benzyl cyanide with potassium hydrosulfide 9 from benzyl cyanide with sodium peroxide 10 by electrolytic reduction of benzyl cyanide in sodium hydroxide 11 from ethyl phenyl-acetate with alcoholic 12 or aqueous 13 ammonia from phenyl-acetic acid with ammonium acetate 14 or urea 15 from diazoacetophenone with ammoniacal silver solution 16 from phenyl-acetic acid imino ether hydrochloride and water 17 from acetophenone with ammonium poly sulfide at 215° 18 from benzoic acid 19 and by heating the ammonium salt of phenyl-acetic acid.20... 

Poly(arylene ether)s containing phenylimidazole units were initially prepared from the reaction of 2-phenyl-4,5-di(4-hydroxyphenyl)imidazole and various activated aromatic difluoro compounds according to Eq. (4) [20]. The dihydroxyimidazole was first prepared from the reaction of 4,4 -dimethoxyben-zil, benzaldehyde and ammonium acetate in refluxing acetic acid followed by... 

Further work on poly(arylene ether phenylimidazole)s led to a series of polymers containing two phenylimidazole units per mer unit (Eq. (5)) [24]. The dihydroxy monomers, 2,2 -(l,3- and l,4-phenylene)bis[(4-phenylhydroxy)-5-phenylimidazole] were prepared from the reaction of iso or terephthaldehyde, 4-hydroxybenzil and ammonium acetate in refluxing acetic acid. High molecular weight polymers as represented in Table 6 were readily prepared in DMAc. 

ACN, acetonitrile MeOH, methanol EtOH, ethanol PrOH, propanol BuOH, butanol EtOAc, ethyl acetate ether, diethyl ether pet. ether, petroleum ether HOAc, acetic acid DCM, dichloromethane THF, tetrahydrofuran TEA, triethylamine DMF, dimethylformamide TFA, trifluoroacetic acid TCA, trichloroacetic acid EDTA, ethylenediaminetetraacetic acid contg, containing soln, solution phosph., phosphate amm., ammonium. 

P-methoxypropionitrile (Fajen, 1985a), furfural and aqueous cuprous ammonium acetate (United States Occupational Safety and Health Administration, 1990b). Stabilizers are commonly used to prevent formation of peroxides in air and polymerization. No information was available on these other exposures, or on exposures to chemicals other than butadiene that are produced in some facilities, such as butylenes, ethylene, propylene, polyethylene and polypropylene resins, methyl-tert-butyl ether and aromatic hydrocarbons (Fajen, 1985b,c). 

Catalyst, alumina, 34, 79 35, 73 ammonium acetate, 31, 25, 27 boron trifluoride etherate, 38, 26 copper chromite, 31,32 36, 12 copper powder in quinoline for pyrolytic decarboxylation,... 

FAB ionization has been used in combination with LC/MS in a technique called continuous-flow FAB LC/MS (Schmitz et al., 1992 van Breemen et al., 1993). Although any standard HPLC solvent can be used, including methyl-ferf-butyl ether and methanol, the mobile phase should not contain nonvolatile additives such as phosphate or Tris buffers. Volatile buffers such as ammonium acetate are compatible at low concentrations (i.e., <10 mM). Continuous-flow FAB has also been used in combination with MS/MS (van Breemen et al., 1993). The main limitationsof continuous-flow FAB compared to other LC/MS techniques for carotenoids, such as ESI and APCI, are the low flow rates and the high maintenance requirements. During use, the 3-nitrobenzyl alcohol matrix polymerizes on the continuous-flow probe tip causing loss of sample signal. As a result, the continuous-flow probe must be removed and cleaned approximately every 3 hr. 

Fraction A was obtained by a 2/1 mixture of chloroform and 2-propanol, fraction B was recovered using 2% acetic acid in ether, fraction C was eluted by methanol, and fraction D resulted from elution by a 420/350/100/50/0.5 mixture of hexane, 2-propanol, ethanol, 0.1 M aqueous ammonium acetate and formic acid. 

Organic acids were separated on a LiChrosorb RP-18 (250-mm X 4.6-mm-ID) column, using the mobile phase 0.005 M ammonium acetate-acetic acid-acetonitrile, at a detection wavelength of 225 or 232 nm. This method can be used for vegetable oils, meat salads, jams, mayonnaise, and mustard (69). After derivatization (benzoylation), it is possible to separate EsHBA with either normal-phase or reverse-phase columns. The normal-phase method showed high efficiency and sensitivity at a detection limit of 0.2 ppm. The preservatives were separated on a LiChrosorb Si 60 column and eluted with isoacetate-diethyl ether-acetonitrile (500 35 0.3). On an RP-18 column, a methanol-water mobile phase was used. Eluents were monitored at 240 nm (70). 

The synthetic procedure developed by Usyatinsky involves pre-absorbing the mixture of acidic support and ammonium acetate (ammonia source) with an ether solution of the starting materials, evaporating the solvent and heating the solid residue in a domestic microwave oven for 20 min (Scheme 5.21). After irradiation, the reaction mixture was allowed to cool to room temperature and was then washed with a mixture of acetone and triethylamine to extract the product from the solid support. No yields were quoted but the purities of the products were quoted to be 75-85%. 

Japanese researchers reacted valerolactim ethers with diethyl ethoxy-methylenemalonate in the presence of ammonium acetate and obtained 6,7,8,9-tetrahydro derivatives of the ester (71 R = H, 6-Me).183... 

The phenethylamine homologue of TMA-6 is well known, but is virtually unexplored pharmacologically. The above benzaldehyde with nitromethane in glacial acetic acid containing ammonium acetate gave the appropriate beta-nitrostyrene as yellow crystals with a mp 177-177.5 °C. This, with LAH in ether, gave 2,4,6-trimethoxyphenethylamine (2,4,6-TMPEA, or 2C-TMA-6) as the picrate salt (mp 204-205 °C) or the hydrochloride salt (mp 234-235 °C). It has been shown not to be a substrate to the soluble amine oxidase from rabbit liver, a property it shares with mescaline, but whether it is or is not active in man is at present unknown. 

Aldehyde or ketone (3 mmol), ammonium acetate (3 mmol, 231 mg), basic alumina (3 g) and active methylene compound 2 (3 mmol) were mixed thoroughly in a mortar. The reaction mixture was placed in a beaker and irradiated under the conditions shown in Table. The progress of reaction was monitored by TLC using petroleum ether-CH2Cl2 (30 70) as eluent. The mixture was extracted into CH2C12 then filtered and washed with water. The solvent was removed under reduced pressure by rotatory evaporator. Further purification by column chromatography on silica gel gave the desired product. 

A mixture of phenyl acetaldehyde 1 (0.6 g, 5 mmol) and morpholine 2a (0.48 g, 5.5 mmol) was placed in a small beaker and irradiated in an unmodified household microwave oven at its full power (900 W) for 2 min. Salicylaldehyde 4a (0.61 g, 5 mmol) and ammonium acetate (0.02 g, 0.25 mmol) were then added to the same reaction vessel, and the reaction mixture was further irradiated in the microwave oven at its 50% power for 5 min using a pulse technique. Upon completion of the reaction, followed by TLC, the reaction mixture was passed through a bed of basic alumina using hexane-ether (9 1, v/v) as an eluent to afford pure 2-aminomorpholinoisoflav-3-enes 6a (yield 80%, mp 103-105 °C). 

A mixture of acidic alumina (9.3 g) and ammonium acetate (4.4 g) was ground in a mortar until a homogeneous powder was formed. A solution of 0.5 mmol of 1,2-dicarbonyl compound and 0.5 mmol of aldehyde in 2 mL of diethyl ether or... 

The Ugi-4CR provides straightforward access to precursors of the pyrazine ring that are suitable for a Davidson cyclization [72], The reaction between arylglyoxals, amines, isocyanides, and benzoylformic acid in ether afforded adducts 114, which cyclized on treatment with an excess of ammonium acetate in acetic acid to give pyrazine carboxamides 115 (Scheme 2.41). 

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