Ammonia chloroform solution

Reaction with chlorosulphonic acid ( chlorosulphonyl-ation ). Sulphonamides. Many aryl hahdes, either alone or in chloroform solution, when treated with excess of chlorosulphonic acid afford the corresponding sulphonyl chlorides in good yield (compare Section IV.106) the latter may be readily converted into the aryl sulphonamides by reaction with concentrated ammonia solution or with sohd ammonium carbonate. 

Evaporate the dried chloroform solution to a residue, add to the residue 400 ml of liquid ammonia, stir and allow the excess ammonia to evaporate, triturate the residue with hexane to form a crystalline solid, continue trituration with water, and filter the solid to yield substantially pure 2-sulfamyl-4-chloro-nitrobenzene. Recrystallize from aqueous methanol. 

Upon adding concentrated ammonia in excess, the condensation product separates and is taken up in chloroform. The chloroform solution is dried and distilled, the tropic acid N-ethyl-N-(7-picolyl)-amide being thereby obtained in the form of a thick oil, which crystallizes after prolonged time and which then melts at 96° to 97°C. 

Procedure. To 10 mL of a solution (Note 2) containing from 1 to 10 pg of nickel(II) add 5mL of a phthalate or acetate (ethanoate) buffer of pH 6.0 or, if the sample solution is acidic, use dilute ammonia to adjust the pH. To this solution now add 15mL of a chloroform solution of dithizone (7 x 10-5M) and 1,10-phenanthroline (3 x 10-5M). Shake the phases for five minutes in a... 

The organic phase was evaporated and the residue dissolved in chloroform. A portion of the chloroform solution was spotted on silica gel plates which were then developed in chloroform methanol ammonia (89 10 1). After development, the plate was air dried and sprayed with a 2M aqueous solution of ammonium bisulfate. After the plate was air dried for 1 hour, the fluorescent spot representing triprolidine was quantitated with a spectrodensitometer in the reflectance mode with 300 nm excitation and emission above 405 nm. With... 

R> = Me, R = R3 = Ph, K = H, R = N=CHAr), which with ammonia in chloroform solution give novel derivatives (224) of meso-ionic l,2,4-triazol-3-imines (216). These compounds are of interest in that they belong to a new type of meso-ionic heterocycle in which the exocyclic substituent f (see Table I) is a stabilized carbanionoid residue,... 

The corresponding ammonium salts are obtained from the quinine salts by treating them with ammonia in an alcoholic chloroform solution. They are viscous substances with rotation of an 425. On mixing equivalent quantities of the two active salts in solution a crystalline racemate is produced. Alkali or alkali carbonates decompose the salts, so that the sodium or potassium salt cannot be produced by decomposing the quinine salts with these reagents. 

When ammonia and sulphur monochloride, S2Cla, each in ice-cold chloroform solution, are mixed, the main course of the reaction is ... 

Sulphamide, SOa(NH2)2, the amide of sulphuric acid, may be obtained by the action of dry ammonia upon a cooled solution of sulphury chloride in either ethylene chloride or chloroform solution 1... 

Sulphimide, or Trisulphimide, (S02NH)s.—This is formed together with ammonia and imidosulphonic acid when sulphamide is heated at 200° to 210° C. It is also formed in small quantity as the ammonium salt, together with sulphamide, when sulphuryl chloride is treated with ammonia in chloroform solution 4... 

Carelli et al., on the other hand, elaborated a basic (rather than an acidic) fractionation scheme to collect the PL present in a chloroform solution of 50-150 mg of sunflower oil most triglycerides were recovered from a 500 mg of bonded diol SPE cartridge using 2.5 ml of chloroform, whereas PL were obtained by elution with 7 ml of methanol containing 0.5 ml/100 ml of a 25% ammonia solution (34). Using this procedure, the recovery of more than 98% pure soybean PE, PA, PI, and PC standards ranged from 94% to 107% at concentrations of 0.1, 0.6, and 1.0% in purified sunflower oil the coefficient of variation was typically of the order of magnitude of 5%. 

Toluene-pyridine—2-chloroethanol-0.8 N ammonia solution Toluene-pyridine - 2-chloroethanol- 25% ammonia Chloroform-benzyl alcbhol-glacial acetic acid Chloroform-rerr.-pentanol-glacial acetic acid Benzene-pyridine-glacial acetic add Chloroform-methanol-gladal acetic acid Chloroform-methanol-glacial acetic add 1 3 6 6 50 15 35 7 70 30 3 70 30 3 40 10 1 95 5 1 14 6 1 17,19,20... 

Evaporate the dried chloroform solution to a residue, add to the residue 400 ml of liquid ammonia, stir and allow the excess ammonia to evaporate, triturate the residue with hexane to form a crystalline solid, continue trituration with water, and filter the solid to yield substantially pure 2-sulfamyl-4-chloro-nitrobenzene. Recrystallize from aqueous methanol. Mix together 4.4 grams of ammonium chloride, 18 ml of methanol, 9 ml of water and 3.0 grams of 2-sulfamyl-4-chloro-nitrobenzene. Heat the mixture to reflux. Add portionwise 4.4 grams of iron filings during a period of about IV2 hours. Cool the mixture and filter. Concentrate the filtrate to a residue. Triturate the residue with 15 ml of water and filter the solid. Recrystallize the solid from aqueous methanol to yield substantially pure 2-sulfamyl-4-chloroaniline. 

To 20% solution of phosgene in toluene, agitated and cooled to 0°C, are added over 30 min a solution of l-p-fluoro-benzoyl-l-hydroxy-3-N-[N -(2-methoxyphenyl)]piperazinopropane and triethylamine in anhydrous chloroform. It is agitated at ambient temperature for 5 h, cooled to 0°C and the solution saturated with gaseous ammonia. The solution is agitated at ambient temperature for 3 h, filtered and the filtrate dried under reduced pressure, 4-p-fluorophenyl-5-p-(4-o-methoxyphenylpiperazino)ethyl-4-oxazolin-2-one, melting point 154°C (by alcohol) was obtained. 

Mercury bis[benzenetellurolate] and sodium benzenetellurolale in liquid ammonia formed a tris[benzenetcllurolato]mercurate(II) anion that was isolated as the tetraphenylphos-phonium salt. This salt and tetraphenylphosphonium benzenetellurolate combined in chloroform solution to give the tetraphenylphosphonium salt of undecakis[benzenetellur-olato ] trimercurate1. 

Procedure (Note Refer to Lead Limit Test, Appendix TTTR, for the solutions and the control.) Add 3 mL of Ammonium Citrate Solution and 0.5 mL of Hydroxylamine Hydrochloride Solution to the Sample Solution, and make the combined solutions alkaline to phenol red TS with ammonium hydroxide. Add 10 mL of Potassium Cyanide Solution. Immediately extract the solution with successive 5-mL portions of Dithizone Extraction Solution, draining off each extract into another separator, until the last portion of dithizone solution retains its green color. Shake the combined extracts for 30 s with 20 mL of 1 100 nitric acid, and discard the chloroform layer. Add exactly 4 mL of Ammonia-Cyanide Solution and 2 drops of Hydroxylamine Hydrochloride Solution to the acid solution. Add 10 mL of Standard Dithizone Solution, and shake the mixture for 30 s. Filter the chloroform layer through an acid-washed filter paper into a Nessler tube, and compare the color with that of a standard prepared as follows Add 0.25 mL of the Standard Lead Solution containing 10 p,g/mL of lead (Pb) ion, 4 mL of Ammonia-Cyanide Solution, and 2 drops of Hydroxylamine Hydrochloride Solution to 20 mL of 1 100 nitric acid, and shake for 30 s with 10 mL of Standard Dithizone Solution. Filter through an acid-washed filter paper into a Nessler tube. The color of the Sample Solution does not exceed that in the control. 

If the methanol solution has been acidified, dilute it with about ten volumes of water, make alkaline with dilute ammonia solution, extract with two 5-ml portions of chloroform, and evaporate the combined chloroform solutions to dryness. The residue is retained for chromatographic examination. 

Iconomou et al.10 determined the ephedrine content in cough syrup and extracted it with chloroform after basification of the syrup with ammonia. The chloroformextract was evaporated and the residue dissolved in a chloroform solution containing the internal standard, diphenyl. Chromatograms of ephedrine-diphenyl solutions (0.1 ya/ul diphenyl) on a 2 m long packed 2 % Versamide 900 on Chromosorb W column with 5 % KOH at 175°C are given i Figure 13.3. 

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