Ammonium, -diethyl chloride

Solid-phase extraction of various analyte complexes on e.g. microcrystalline naphthalene (Ni [23] and Cu [24] with nitroso-R salt and tetradecyldimethylbenzylammonium chloride), ammonium tetraphenylborate-naphthalene (U with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol) [25], chitin column (Cr(VI) with 1,5-diphenylcarbazide) [26], strong anion-exchange cartridge (Cr(VI) at pH 8) [27], Cig cartridge (CL-azo dye) [28] and minicolumn (As with ammonium diethyl dithiophosphate) [29], silica modified chemically with A-allyl- or A-phenyl-TV -propylthiourea (OSO4) [30] and Sephadex DEAE A-25 (chloride form) (V with Eriochrome Cyanine R) [31] prior to the spectrophotometric determination has recently been reported. The application of solid-phase spectrophotometry to determine nitrite and nitrate in water samples has recently been described [32]. 

AI3-52461 Ammonium, (6-(diethylamino)-3H-xanthen-3-ylidene)diethyl-, chloride Ammonium, diethyl(6-(dielhyl-amino)-3H-xanthen-3-ylidene)-, chloride 3,6-Bis(diethyl-amino)xanthylium chloride C.l. 45010 (6-(Diethyl-amino)-3H-xanthen-3-ylidine)dielhylammonium chloride N-(6-(Diethylamino)-3H-xanthen-... 

Ammonium, (carboxymethyl) dodecyidimethyl-, hydroxide, inner salt. See Lauryl betaine Ammonium, (carboxymethyl) trimethyl-, chloride. See Betaine hydrochioride Ammonium, (9-(o-carboxyphenyl)-6-(diethylamino)-3H-xanthen-3-ylidene) diethyl-, chloride. See Basic vioiet 10 D C Red No. 19 Ammonium, (3-carboxypropyl) trimethyl-, chloride, methyl ester. See Carpronium chloride... 

Ammonium, didecyidimethyl-, chloride. See Didecyidimonium chloride Ammonium, (4-(p-(diethylamino)-a-phenylbenzylidene)-2,5-cyclohexadien-1-ylidene) diethyl-, sulfate (1 1). See Basic green 1... 

Now run in a solution of 52 g. (53-5 ml.) of pure diethyl carbonate (1) in 70 ml. of anhydrous ether, with rapid stirring, over a period of about one hour. A vigorous reaction sets in and the ether refluxes continually. When the diethyl carbonate has been added, heat the flask on a water bath with stirring for another hour. Pour the reaction mixture, with frequent shaking, into a 2 litre round-bottomed flask containing 500 g. of crushed ice and a solution of 100 g. of ammonium chloride in 200 ml. of water. Transfer to a separatory funnel, remove the ether layer, and extract the aqueous solution with two 176 ml. portions of ether. Dry... 

To a solution of 0.30 mol of ethyllithium (note 1) in about 270 ml of diethyl ether (see Chapter II, Exp. 1) v/as added 0.30 mol of methoxyallene at -20°C (see Chapter IV, Exp. 4) at a rate such that the temperature could be kept between -15 and -2Q°C. Fifteen minutes later a mixture of 0.27 mol of >z-butyl bromide and 100 ml of pure, dry HMPT ivas added in 5 min with efficient cooling, so that the temperature of the reaction mixture remained below 0°C. The cooling bath was then removed and the temperature was allowed to rise. After 4 h the brown reaction mixture was poured into 200 ml of ice-water. The aqueous layer was extracted twice with diethyl ether. The combined solutions were washed with concentrated ammonium chloride solution (which had been made slightly alkaline by addition of a few millilitres of aqueous ammonia, note 2) and dried over potassium carbonate. After addition of a small amount (2-5 ml) of... 

A solution of a-lithiomethoxyallene was prepared from nethoxyal lene and 0.20 mol of ethyllithiurn (note 1) in about 200 ml of diethyl ether (see Chapter II, Exp. 15). The solution was cooled to -50°C and 0.20 mol of ethylene oxide was added immediately. The cooling bath was removed temporarily and the temperature was allowed to rise to -15 c and was kept at this level for 2.5 h. The mixture was then poured into 200 ml of saturated ammonium chloride solution, to which a few millilitres of aqueous ammonia had been added (note 2). After shaking the layers were separated. The aqueous layer was extracted six times with small portions of diethyl ether. The combined ethereal solutions were dried over sodium sulfate and subsequently concentrated in a water-pump vacuum. Distillation of the... 

The solution was then poured into 200 ml of saturated ammonium chloride solution. After vigorous shaking the upper layer was separated off and the aqueous layer was extracted three times with diethyl ether. The combined ethereal solutions were dried over magnesium sulfate and then concentrated in a water-pump vacuum. 

To a solution of 0.40 mol of butyllithium in about 280 ml of hexane were added 280 ml of dry THF with cooling below -10°C. Subsequently 0.40 mol of 1,1-diethoxy--2-propyne (see Chapter V, Exp. 28) was introduced in 15 min at -30 to -10°C. To the solution obtained was then added in 15 min with cooling at about -15°C 0.40 mol of chloromethyl ethyl ether (note 2). After the addition stirring was continued for 1 h without cooling. The mixture was then shaken with concentrated ammonium chloride solution and the ethereal layer was separated off. The aqueous layer was extracted twice with diethyl ether. After drying the ethereal solutions over magnesium sulfate the diethyl ether was evaporated in a water-pump vacuum. 

A solution of 0.22 mol of butyllithium in 150 ml of hexane was cooled below -40°C and 140 ml of dry THF were added. Subsequently 0.20 mol of 1-dimethyl amino--4-methoxy-2-butyne (see Chapter V, Exp. 14) were added in 10 min with cooling between -35 and -45°C. After an additional 15 min 100 ml of an aqueous solution of 25 g of ammonium chloride were added with vigorous stirring. After separation of the layers four extractions with diethyl ether were carried out. The solutions were dried over potassium carbonate and then concentrated in a water-pump vacuum. Distillation of the residue gave a mixture of 8-10% of starting compound and 90-92% of the allenic ether, b.p. 50°C/12 mmHg, n 1.4648, in 82% yield (note 1). 

To a solution of 0.40 mol of butyllithium in about 280 ml of hexane were added 300 ml of dry THF at -20 to -40 0. Subsequently 0.40 mol of freshly distilled tert.-butyl propargyl ether was added, keeping the temperature below -30°C. Freshly distilled acetaldehyde (0.40 mol) was then added at the same temperature during about 15 min. The cooling bath was removed and, after an additional 15 min, 200 ml of an aqueous solution of 30 g of ammonium chloride were introduced. After separation of the layers the aqueous layer was extracted twice with diethyl ether and the combined solutions were dried over magnesium sulfate and concentrated in... 

To a solution of 0.25 mol of the trimethylsilyl ether in 120 ml of dry diethyl ether was added in 20 min at -35°C 0.50 mol of ethyllithium in about 400 ml of diethyl ether (see Chapter II, Exp. 1). After an additional 30 min at -30°C the reaction mixture was poured into a solution of 40 g of ammonium chloride in 300 ml of water. After shaking, the upper layer was separated off and dried over magnesium sulfate and the aqueous layer was extracted twice with diethyl ether. The ethereal solution of the cumulenic ether was concentrated in a water-pump vacuum and the residue carefully distilled through a 30-cm Vigreux column at 1 mmHg. The product passed over at about 55°C, had 1.5118, and was obtained in a yield of 874. Distillation at water-pump pressure (b.p. 72°C/I5 mmHg) gave some losses due to polymerization. 

The mixture was hydrolysed by gradually adding (with vigorous stirring) a solution of 20 g of ammonium chloride and 3 g of NaCN or KCN in 150 ml of water. After separation of the layers, two extractions with diethyl ether were carried out. 

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