Amine decanters

Diallyl amine (7V-2-propenyl-2-propen-l-amine) [124-02-7] M 97.2, b 107-lll /760mm, 112 /760mm, dj 0.789, Dp 1.440, pK 9.42. Keep over KOH pellets overnight, decant and distil from a few pellets of KOH at atm pressure (b 108-111 ), then fractionate through a Vigreux column. [Vliet J Am Chem Soc 46 1307 7924 Org Synth Coll Vol I 201 1941.] The hydrochloride has m 164-165 (from Me2CO + EtOH). [Butler and Angels J Am Chem Soc 79 3128 1957.]... 

Products from the reactor are recovered in the main fractionator a J the gas plant. The main fractionator recovers the heaviest produc, such as light cycle and decanted oil, from the gasoline and ligh r products. The gas plant separates the main fractionator overhead vap< s into gasoline, Cj s, C4 s and fuel gas. The products contain sulfur compounds and need to be treated prior to being used. A combination of amine and caustic solutions are employed to sweeten these products... 

Silica Alkylation. To tetiamethyldisihzane (TMDS, 1.0 g) in anhydrous toluene (30 mL), amine-functionalized silica was added and stirred overnight at room temperature under N2. Then it was then filtered, washed with toluene three times, and dried under vacuum at 50°C. Ethanol (190 mL) and nanopure water (10 mL) were mixed, and the pH was adjusted to 4.7 with acetic acid. Isobutyltrimethoxysilane (4.0 mL) was added to the solution, stirred for five minutes, and the modified silica was added. After 10 minutes, the solution was decanted, the... 

Filter, wash toluene with water, NaHC03, water and dry, evaporate in vacuum to get 100 g gamma-Cl-butyraldehyde (I) (can distill 28/2). 10 g (I), 20 g 3-nitro-phenylhydrazine dissolve in the minimum volume of hot ethanol containing 10% glacial acetic acid. Heat on steam bath one hour cool and add water until dark oil separates. Evaporate in vacuum the ethanol and decant the water to get the oily gamma-Cl-butyraldehyde-3-intro-phenylhydrazone(II). 29 g (11), 300 ml concentrated HC1, ZOO ml benzene stir three hours, replace benzene with fresh benzene and stir four hours. Combine the two benzene portions, wash with water and dry, evaporate in vacuum to get 4 g 3-(beta-Cl-ethyl)-4 and 6-nitroindole (m). 3.56 g (III), 200 ml ethanol, 200 ml 34% aqueous DMA (or other amine) and let stand at room temperature for one week. Evaporate in vacuum the ethanol, filter, dissolve the precipitate in dilute HC1 and filter. Basify the filtrate with dilute NaOH to precipitate 3 g 4 and 6-nitro-DMT (IV). 5.2 g (IV), 350 ml ethanol, 100 ml IN NaOH heat to 50° and add a solution of 3 g Na dithionite in 15 ml 0.2N NaOH. filter hot and evaporate in vacuum to get 2 g 4 and 6 amino-DMT (can purity by dissolving in HC1, filter, basify, extract with ether and dry and evaporate in vacuum the extract). 

The dinitro product is then cooled and filtered (the spent acid hquor is recoverable), the cake is washed with water, and the resulting washwater is sent to the wastewater treatment plant. The dinitro compound is then dissolved in an appropriate solvent and added to the amination reactor with water and soda ash. An amine is then reacted with the dinitro compound. The crude product is passed through a filter press and decanter and finally vacuum distilled. The saltwater layer from the decanter is discharged for treatment. The solvent fraction can be recycled to the reactor, and vacuum exhausts are caustic scrubbed. Still bottoms are generally incinerated. 

Ethylenediamine (en) [15] Among the impurities are water, carbon dioxide, ammonia and polyethylene amines (e.g. diethylenetriamine and triethylenetetra-mine). In the recommended purification method, commercial product (98%) is shaken for about 12h with activated molecular sieves (5A, 70 gl-1), the supernatant is decanted and shaken for about 12 h with a mixture of CaO (50 gl-1) and... 

This ketone (114mg, 0.106mmol) in EtOAc (2mL) was cooled to —30°C. Gaseous HC1 was then introduced so as to maintain the temperature between —10 and — 20 °C. The soln was kept at this temperature for 2h, then at 0°C for 4h. It was purged with N2 for 30 min at 0°C. The soln was concentrated, and the residue was triturated and washed by decantation with tBuOMe/hexane (1 4, 3x2 mL). The product was collected and dried to give the amine salt yield 81 mg (90%). 

If a large aqueous phase appears, the amine should be decanted and dried further over a fresh portion of potassium hydroxide pellets. 

The Schotten-Baumann method of benzoylation with benzoyl chloride in the presence of aqueous sodium hydroxide may be used. Full details are given under Primary and secondary amines, Section 9.6.21, p. 1273. Alternatively, dissolve 1.0 g of the phenol in 3 ml of dry pyridine and add 0.5 g of benzoyl chloride. After the initial reaction has subsided, warm the mixture over a small flame for a minute or two and pour, with vigorous stirring, into 10-15 ml of water. Allow the precipitate to settle, decant the supernatant liquid, stir the residue thoroughly with 5-10 ml of m sodium carbonate solution, filter and recrystallise from ethanol or from light petroleum. 

The mixture was then treated with 5 ml of alkaline hydroxyl-amine reagent ( 20 ml hydroxylamine hydrochloride titrated to pH 13 with 3.5M NaOH ) for 5 min and the protein precipitated with 5% trichloroacetic acid. After centrifuging ( 5000 g ) for 5 min the supernatant was carefully decanted and the precipitate washed twice with 10-ml aliquots of absolute ethanol. The material was then dissolved in 1 ml, of 0.2M NaOH, mixed with 10 ml of Insta-gel scintillator ( Packard Instrument (Pty) Ltd.), and the radioactivity counted in a Packard Tri Carb Liquid Scintillation Spectrometer. 

A solution of N-(4-pyridinyl)-lH-indol-l-amine (6 g) in 25 ml of dimethylformamide was slowly added to an ice-cooled suspension of NaH (1.3 g of 60% NaH dispersion in mineral oil was washed with hexanes, the liquid was decanted and the residual solid was dispersed in 5 ml of dimethylformamide). After anion formation, a solution of 1-bromopropane (4 g) in 5 ml of dimethylformamide was added. After one hour of stirring at ambient temperature, the reaction mixture was stirred with ice-water and extracted with dichloromethane. The organic extract was washed with water and saturated sodium chloride solution, was dried over anhydrous magnesium sulfate, filtered and concentrated to 8 g of oil. This oil was purified by HPLC (silica, ethyl acetate) and thereafter by column chromatography (alumina, ether) to give 6.4 g oil. This oil was converted to the maleate salt and recrystallized from methanol/ether to give 6.8 g of crystals, m.p. 115-116°C. 

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