Ethanol extraction with

Nguyen et al. (1991) extracted ole-oresin from vanilla beans with 2—62 g C02/g dried bean at 306—309 K and 10-13 MPa. Vanillin yields of up to 95% were attained. Vanillin purity was higher with supercritical C02 extraction than with conventional aqueous ethanol extraction, with vanillin representing 74-97% of the flavour and fragrance compounds, compared with 61% using alcohol extraction. 

Improved mass transfer leads to smaller extraction equipment with shorter residence times. Weatherley et al.52 studied ethanol extraction with decanol under a range of electrically enhanced experimental conditions. 

Vatai G and Tekic MN, Membrane-based ethanol extraction with hollow fiber module. Separation Science and Technology 1991, 26(7), 1005-1011. 

Cetyltrimethylammonium bromide (CTMABr) was dissolved in water at 40°C, a clear micellar solution was obtained. Then sodium silicate was added to this solution and the pH value was adjusted with sulfuric acid. pH value and surfactant/silicium molar ratio were fixed at 10 and 0.62 respectively according to literature [8], After stirring for several hours at room temperature, the homogenous gel with the molar composition of 1 CTMABr 0.63 SiOz 102 HzO was sealed in Teflon autoclaves and heated. The crystallization temperature and time varied respectively from 80°C to 140°C and from 1 day to 11 days. The obtained solid phases after ethanol extraction with a Soxhlet apparatus were dried in vacuum at 100 °C overnight. 

Dry gaseous sulfur trioxide was bubbled through a solution of triphenylbismuthine (10 g, 22.7 mmol) in 1,2-dichloroethane (40 ml) for 2 h at — 10°C. On addition of ether (400 ml), a white precipitate was formed. This was filtered off and extracted with dry ethanol (3 ml X 50). Dilution of the combined ethanol extracts with petroleum ether (b.p. ca. 40°C) gave a white solid, which was filtered off, washed with ether, and dried to give diphenylbismuth benzenesulfonate (3.2 g, 27%) [861CA(113)43]. 

Extract with DCM. Concentrated and loaded onto a dual-stage carbon sorbent trap. SPED Extract with DCM or solid-phase extraction on two adsorbents (C8 and activated carbon), and elute with ethanol Extract with DCM. Wastewater (CLLE)... 

Recently, Shahidi et al. [31] found that total antioxidant activity of hazelnut extracts ranged from 29 to 148 xmol TE/g of ethanolic extract, with lowest activity in hazelnut kernel aud highest in hazelnut tree leaf (Table 13.1). The total antioxidaut activity of hazelnut by-product extracts were approximately 4-to5-fold higher than that of hazelnut kernel at the same extract concentration. At a given concentration, hazelnut by-product extracts would serve as a more effective antioxidant than hazelnut kernel extract. Consideration of defatted hazelnut (on an extract basis) and hazelnut (as is weight basis) make the quantitative comparison between the studies of Wu et al. [4] and Shahidi et al. [31] impossible. 

In the case of ethanol, extraction with water is undesirable due to the dilution of the ethanol, whereas direct pressing gives poor yields [184]. Direct distillation from the fermented solids performs relatively poorly, although distillation is economically feasible if combined with animal feed production from the solid wastes [217,218]. As an alternative, forced gas circulation can be used to strip ethanol from the substrate. This has been shown for a gas-solid fluidized bed and for a stirred bed [90, 219, 220]. A further advantage is that continuous stripping during the fermentation, rather than simply recovering the ethanol at the end of the fermentation, avoids the product inhibition... 

Preparative TLC and high-resolution (HR) EI-MS were used for isolation of santolinoic acid, a new ursane-type triterpenoid, from Salvia santolinifolia [31]. Partitioning of the ethanolic extract with different solvents was followed by column... 

A certain amount of hydrolysis of the original acetamide to acid and ammonia always occurs, and the final amine always contains traces of ammonia. This is separated by extracting the mixed anhydrous hydrochlorides with absolute ethanol, which dissolves the amine hydrochloride but not the ammonium chloride filtration of the hot ethanolic extract removes the ammonium chloride, whilst the amine hydrochloride crystallises readily from the filtrate on cooling. 

For alcohols of b.p. below 150°, mix 0- 5 g. of 3-nitrophthalic anhydride (Section VII,19) and 0-5 ml. (0-4 g.) of the dry alcohol in a test-tube fitted with a short condenser, and heat under reflux for 10 minutes after the mixture liquefies. For alcohols boiling above 150°, use the same quantities of reactants, add 5 ml. of dry toluene, heat under reflux until all the anhydride has dissolved and then for 20 minutes more remove the toluene under reduced pressure (suction with water pump). The reaction product usually solidifies upon cooling, particularly upon rubbing with a glass rod and standing. If it does not crystallise, extract it with dilute sodium bicarbonate solution, wash the extract with ether, and acidify. Recrystallise from hot water, or from 30 to 40 per cent, ethanol or from toluene. It may be noted that the m.p. of 3-nitrophthalic acid is 218°. 

Method 1. Reflux a mixture of pure nicotinic acid (Section V,22), 84 g. (105 ml.) of absolute ethanol and 90 g. (50 ml.) of concentrated sulphuric acid in a flask for 4 hours on a steam bath. Cool the solution and pour it slowly and with stirring on to 200 g. of crushed ice. Add sufficient ammonia solution to render the resulting solution strongly alkaline generally, some ester separates as an oil but most of it remains dissolved in the alkaline solution. Extract the solution with five 25 ml. portions of ether, dry the combined ethereal extracts with anhydrous magnesium sulphate, remove the ether and distil under reduced pressure. The ethyl nicotinate passes over at 117-118°/ 6 mm. the yield is 34 g. The b.p. under normal pressure is 222-224°. 

In a typical experiment 105 mg (0.50 mmol) of 3.8c, dissolved in a minimal amount of ethanol, and 100 mg (1.50 mmol) of 3.9 were added to a solution of 1.21g (5 mmol) of Cu(N03)2 BH20 and 5 mmol of ligand in 500 ml of water in a 500 ml flask. -Amino-acid containing solutions required addition of one equivalent of sodium hydroxide. When necessary, the pH was adjusted to a value of 5 ( -amino acids) and 7.5 (amines). The flask was sealed carefully and the solution was stirred for 2A hours, followed by extraction with ether. After drying over sodium sulfate the ether was evaporated. Tire endo-exo ratios were determined from the H-NMR spectra of the product mixtures as described in Chapter 2. 

In a typical procedure, a solution of 0.175 mmol of L- -amino acid and 0.175 mmol of NaOH in 1 ml of water was added to a solution of 0.100 mmol of Cu(N03)2in 100 ml of water in a 100 ml flask. Tire pH was adjusted to 6.0-6.5. The catalyst solution was cooled to 0 C and a solution of 1.0 mmol of 3.8c in a minimal amount of ethanol was added, together with 2.4 mmol of 3.9. The flask was sealed carefully. After 48 hours of stirring at 0 C the reaction mixture was extracted with ether, affording 3.10c in quantitative yield After evaporation of the ether from the water layer (rotary evaporator) the catalyst solution can be reused without a significant decrease in enantioselectivity. 

METHOD 2 [89]--1M MDA or benzedrine and 1M benzaldehyde is dissolved in 95% ethanol (Everclear), stirred, the solvent removed by distillation then the oil vacuum distilled to give 95% yellow oil which is a Schiff base intermediate. 1M of this intermediate, plus 1M iodomethane, is sealed in a pipe bomb that s dumped in boiling water for 5 hours giving an orangy-red heavy oil. The oil is taken up in methanol, 1/8 its volume of dH20 is added and the solution refluxed for 30 minutes. Next, an equal volume of water is added and the whole solution boiled openly until no more odor of benzaldehyde is detected (smells like almond extract). The solution is acidified with acetic acid, washed with ether (discard ether), the MDMA or meth freebase liberated with NaOH and extracted with ether to afford a yield of 90% for meth and 65% for MDMA. That s not a bad conversion but what s with having to use benzaldehyde (a List chemical) Strike wonders if another aldehyde can substitute. 

Ojj 1.5323, prepared from phenol, KOH in ethanol and propargyl bromide) was added and the mixture was heated at 60°C for 15 min. It was then poured into 200 ml of ice-water and the reaction products were extracted with diethyl ether. The ethereal extracts were washed with saturated NH Cl solution, dried over magnesium sulfate and then concentrated in a water-pump vacuum. There remained 9.5 g of 3 1 mixture... 

Bromo-2-nitrophenylacetic acid (26 g, 0.10 mol) was dissolved in a mixture of 50% HjSO (400 ml) and ethanol (600 ml) and heated to 90°C. Over a period of 1 h, zinc dust (26.2 g, 0.40 mol) was added. slowly and then heating was continued for 2 h. The excess ethanol was removed by distillation. The solution was cooled and filtered. The filtrate was extracted with EtOAc. The filtered product and extract were combined, washed with 5% NaCOj and brine and then dried (MgSO ). The solvent was removed in vacuo and the residue recrystallized from methanol to give 20.5 g (97% yield) of the oxindole. 

In the continuous process for producing phosphatidylcholine fractions with 70—96% PC at a capacity of 600 t/yr (Pig. 5) (16), lecithin is continuously extracted with ethanol at 80°C. After separation the ethanol-insoluble fraction is separated. The ethanol-soluble fraction mns into a chromatography column and is eluted with ethanol at 100°C. The phosphatidylcholine solution is concentrated and dried. The pure phosphatidylcholine is separated as dry sticky material. This material can be granulated (17). 

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