Oil purification

Chromatographic purification required for each intermediate, the majority of which were oils Purification options would be limited... 

Upon cooling to room temperature, a gray precipitate forms and the reaction is quenched with 220 mL of saturated, aqueous ammonium chloride. The resulting mixture is poured into a 1-L separatory funnel and extracted with 220 mL of diethyl ether. The organic fraction is washed two times with 100 mL of water, and once with 100 mL of brine, dried over magnesium sulfate, filtered, and concentrated under reduced pressure to provide 44.1 g of crude product as a pale yellow oil. Purification of this material by bulb-to-bulb distillation (140-145°C, 0.5 mm) (Note 11) into a chilled (-78°C) receiving flask yields 41.0 g (92%) of 2 as a clear, colorless oil (Note 12). 

The oil described above was utilized directly in the condensation reaction with the epichlorohydrin. A mixture of 0.1 mole of methyl 3-(4-hydroxyphenyl)propionate, 0.2 mole potassium carbonate and 0.4 mole epichlorohydrin in 250 mL acetone was heated to reflux for 24 hours. The reaction medium was then filtered and evaporated. The residue was taken up in 100 mL toluene and washed with 100 mL 1.0 N NaOH and 100 mL water (2 times). The toluene phase was then dried over magnesium sulfate and evaporated to provide the crude product as an oil. Purification was effected by vacuum distillation (156°C/0.4 mm) and provided methyl 3-[4-(2,3-epoxypropoxy)phenyl]propionate. The NMR and IR spectra and elemental analysis data were consistent with the assigned structure. 

A solution of 14 (2.0 g, 3.8 mmol), 2,3-bis(hydroxyamino)-2,3-dimethylbutane sulfate (4.75 g, 19.3 mmol) and potassium carbonate (2.85 g, 20.6 mmol) in methanol (40 mL) was refluxed for 24 h. The reaction mixture was poured into water, extracted with ethyl acetate, washed with water, dried over magnesium sulfate and concentrated to give tetrahydroxylamine as a yellow oil. Purification was not performed. 

To a solution of Grubbs catalyst G1 (943 mg, 1.15 mmol, 0.4 equiv) in CH2C12 (900 mL) was added a solution of enyne 51 (2.00 g, 2.86 mmol, 1.0 equiv) in toluene (100mL). The reaction was purged with ethylene and stirred at 45 °C under an atmosphere of ethylene for 40 h. The crude mixture was treated with ethyl vinyl ether (1 mL) and concentrated to a black oil. Purification by silica gel chromatography (doped with triethylamine, 5-6% in CH2Cl2/hexane) afforded cyclophane 53 (624 mg, 31%). 

Refrigeration is best known for its use in the air conditioning of buildings and in the treatment, transportation, and preservation of foods and beverages. It also finds large-scale industrial use, for example, in the manufacture of ice and the dehydration of gases. Applications in the petroleum industry include lubricating-oil purification, low-temperature reactions, and separation of volatile hydro-1 carbons. A closely related process is gas liquefaction, which has important commercial applications. 

To a solution of copper chloride (2.4 mg, 0.024 mmol) in DMF (1.5 ml) was added l-chloro-2-phenylacetylene (50 mg, 0.37 mmol) at r.t. To the mixture was added trimethyl(4-methoxyphenylethynyl)silane (50 mg, 0.25 mmol). The reaction mixture was stirred for 48 h at 80 °C, quenched with 3 M HCl, and extracted with diethyl ether (25 ml x 2). The combined ethereal layer was washed with aqueous NaHCOj solution, then with brine and dried over MgS04. Filtration and evaporation provided a brown oil. Purification by column chromatography (Si02, hexane dichloromethane = 10 1) gave l-(4-methoxyphenyl)-4-phenyl-1,3-butadiyne (36 mg, 65% yield) as a colorless solid. 

To a stirred solution of a S-oxo ester 31 (1 mmol) in benzene (80 mL) was added Et N (0.5 mL), and the mixture was stirred at rt for 1 h. Benzene-1,2-diamine (2 mmol) and TsOH (50 mg) were added to the resulting pale-yellow solution, which was then refluxed for 2 h and concentrated in vacuo. The residue was dissolved in EtOAc (80 mL), washed with 1 M aq HCl (50 mL) and sat. aq NaHCO (50 mL), passed through a short pad of MgSO and silica gel 60, and concentrated to provide a pale yellow oil. Purification by flash chromatography (silica gel, hexane/EtOAc 90 10) gave the quiiioxaliiie derivatives as a colorless solid. 

Powdered activated carbon (PAC) can be derived from a number of different agricultural commodities, including waste soy hull (32-36). Commercial activated carbon, however, is manufactured from only a few of these, including wood and sawdust, peat, hgnite, nutshells (including coconut shell), and pits (37). Related materials include animal charcoal, gas black, furnace black, lamp black, and activated charcoal, but these are not used in fats and oils purification and will not be further addressed. 

Activated carbon possesses extremely high surface area (38), often in excess of 1000 m /g. Much of that surface area is, however, associated with micropores—that is, pores <20 A (<2 nm) in diameter. The surface area associated with meso-pores—pores 20 to 500 A (2 to 50 nm) in diameter—is considerably lower (typically in the range 10—100 m /g). Most liquid-based applications (including fats and oils purification) involve the adsorption of high-molecular-weight contaminants whose molecular dimensions prevent penetration into micropores therefore, activated carbon containing significant mesoporosity is most desirable in these applications (39). 

Use Mordant for dyeing, pigments, manufacturing of alizarin, chrome alum, oil purification, pickling, manufacture of catalysts, leather tanning, synthetic perfumes, photography, process engraving and li-... 

Derivation Esterification of ricinoleic acid or alcoholysis of castor oil, purification by vacuum distillation. 

Lipases have also been employed to isolate tocopherols and sterols, important antioxidants from deodorizer distillate, a by-product formed during the deodoriza-tion step of seed oil purification, by hydrolyzing MAG and DAG in the distillate, and by esterifying sterols into sterol esters. The latter serves as antioxidant in non-polar food products such as margarine (e.g., Benacol from the Raisio Group, Finland and Take Control from Unilever, Englewood Cliffs, New Jersey, U.S.A.). PUFA-sterol esters would provide the benefits of essential fatty acid intake and antioxidant protection. 

A solution of Marlin s sulfurane (0.949 g, 1.41 mmol) in CH2CI2 (5 mL) was slowly added under an atmosphere of nitrogen to a stirred solution of the alcohol (0.41 g, 0.94 mmol) in CH2CI2 (10 rnL) at room temperature. The resulting pale yellow solution was stirred for 24 h at which time the solvent was removed in vacuo to yield the crude product as a pale yellow oil. Purification by flash column chromatography [SiO2 EtOAc petroleum ether (40 60)] followed by recrystallization (CH3OH/H2O) furnished the olefin product as a colorless solid (0.33 g, 84% yield). 

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