W-Butanol

C) Mixed solvent. A well-shaken mixture of 20 ml. of redistilled w-butanol, 9-5 ml. of water, and 5-5 ml. of 95% ethanol. 

FIGURE 10.5 Elution profile on OH-B12 treated by microwave heating for 6 min during silica gel 60 column chromatography. Fifty milliliters of the treated OH-B12 solution (5 mmol/1) was evaporated to dryness and dissolved in a small amount of w-butanol/2-pro-panol/water (10 7 10, v/v) as a solvent. The concentrated solution was put on a column (1.4 X 15.0 cm) of silica gel 60 equilibrated with the same solvent and eluted with the same solvent in the dark. The eluate was collected at 4.0 ml with a fraction collector. Fractions I to V were pooled, evaporated to dryness, dissolved with a small amount of distilled water, and analyzed with silica gel TLC. Inset represents the mobile pattern of the OH-B12 degradation products of fractions I to V on the TLC plate. Data are typical, taken from one of five experiments. (Reprinted with permission from Watanabe, F. et al., J. Agric. Food Chem., 46, 5177-5180, 1998. Copyright (1998) American Chemical Society.)... 

A novel reaction for the synthesis of 4-amino-substituted quinolines 80 or 4-quinolones 81 was reported. Reaction of various ketones, such as 82 and 83, with o-oxazoline-substituted anilines 84 and 85 in the presence of a catalytic amount of /Mol ucncsul tonic acid (p-TSA) in dry w-butanol led to 80 and 81, respectively <06T9365>. To the authors surprise, the reaction of acetophenones 82 lead to a different outcome than that of the cyclic or acyclic ketones 83 containing more than one carbons a to the ketone. 

Isolate the biotinylated probe by ethanol/salt precipitation as described in Section 1 (this chapter) for nick-translation modification of DNA probes. Alternatively, dialysis, gel filtration, or w-butanol extraction may be used to remove excess reagents. 

Purify the biotinylated DNA probe by ethanol precipitation, gel filtration, w-butanol extraction, or dialysis as discussed in previous sections. 

Microorganisms have also been developed to produce alternative products, such as lactic acid [65], propane-1,3-diol [67], 3-hydroxypropionic acid [68], butane-2,3-diol [69] and numerous other intermediates. For instance, bacteria such as the Clostridium acetobutylicum ferment free sugars to C4 oxygenates such as butyric acid or butanol. They form the C4 oxygenates by Aldol condensation of the acetaldehyde intermediates. The Weizmann process exploits this property to ferment starch feedstock anaerobically at 37 °C to produce a mixture of w-butanol, acetone and ethanol in a volume ratio of 70 25 5 [3],... 

Alcohols are hydroxylated alkyl-compounds (R-OH) which are neutral in reaction due to their unionizable (OH) group (e.g., methanol, ethanol, isopropanol, and w-butanol). The hydroxyl of alcohols can displace water molecules in the primary hydration shell of cations adsorbed onto soil-solid and sediment-solid clay particles. The water molecule displacement depends mainly on the polarizing power of the cation. The other adsorption mechanisms of alcohol hydroxyl groups are through hydrogen bonding and cation-dipole interactions [19,65],... 

Dry hexane (40 mL) was added to the Humicola sp. lipase BREP prepared above in Procedure 1. This suspension was transferred to a 100 mL round-bottom flask containing the enol acetate 1 (760 mg, 3.92 mmol). Dry w-butanol (0.72 mL, 7.84 mmol) was added and the mixmre stirred at 25 °C for 1 h. 

The most convenient methods to be used with silica having no pores or very wide ones are the reaction with thionyl chloride, the esterification with methanol or w-butanol and higher alcohols, and ion exchange, e.g., with uranyl ions (however, the general applicability of the latter reagent... 

Urea and melamine are tetra- and hexa-functional molecules. However, the formation of a network polymer is prevented by adding alcohols such as w-butanol and by condensing with formaldehyde at low temperatures under basic conditions. While phenol resins have better moisture and weather resistance than urea resins, the latter are preferred for light-colored... 

The recovery of w-butanol from a fermentation broth in a similar way has been investigated by in situ extraction with [BMIMJJPF, ] (Entry 5) [33]. 

During this same time period, ethylene glycol was reported as a product in cobalt-catalyzed methanol homologation reactions methanol, ethanol, and glycol ethers were also found in similar reactions carried out to homologate w-propanol and w-butanol (34). Reaction conditions were 800-1000 atm of H2/CO at 225°C. 

To a flask containing 405 gm (5.47 moles) of w-butanol is added 25.3 gm (1.1 gm-atom) of sodium metal in small portions. After the reaction is complete, 154.0 (1.0 mole) of A V-di-w-butylcyanamide is added with sufficient benzene to keep the refluxing pot temperature at approximately 100°C. The mixture is refluxed for 3 hr, glacial acetic acid is added to neutralize the base, the mixture is washed with water, the organic layer is separated, dried, and then distilled to afford 194.0 gm (85 %), b.p. 117°C (2.0 mm), ng 1.4500, df 0.8871. 

We conclude this section with some brief comments on the cosolvent effects of partially miscible organic solvents (PMOSs). These solvents include very polar liquids such as w-butanol, w-butanone, w-pentanol, or o-cresol, but also nonpolar organic compounds such as benzene, toluene, or halogenated methanes, ethanes, and ethenes. For the polar PMOS, a similar effect as for the CMOS can be observed that is, these solvents decrease the activity coefficient of an organic solute when added to pure water or to a CMOS/water mixture (Pinal et al., 1990 Pinal et al., 1991 Li and Andren, 1994). For the less polar PMOS there is not enough data available to draw any general conclusions. 

Once again the scientist chose to use the SNAr reaction to gain access to the key o-nitroaniline intermediate however, it is quite apparent from Table 8.7 that the use of microwave synthesis resulted in rapid optimization of this key reaction and significantly improved yields. The use of w-butanol as solvent for this substitution reaction gave high yields (88%) in only 15 min. It should also be pointed out that while in the thermal example DMSO was the optimal solvent, in the microwave example this solvent resulted in decomposed starting materials. 

Fractions H and /. Paper chromatography indicated that these two fractions were identical except for a few minor spots. The combined fractions were purified by cellulose column chromatography with the upper layer of 4 1 5 w-butanol-ethanol-water as the developer. Over 95% of the combined fraction was recovered as pure oxalic acid. 

Dissolve the toxin to be conjugated in 0.1 M sodium phosphate, 0.15 M NaCl, pH 7.5, at a concentration of 10 mg/ml. Some protocols use as an SPDP reaction buffer, 50 mM sodium borate, 0.3 M NaCl, 0.5% w-butanol, pH 9. Both buffer systems work well for the NHS ester modification reaction, although the pH 9 buffer is at the higher end of effective derivatization with active esters, since the hydrolysis rate is dramatically increased at this level of alkalinity. 

Immediately extract excess DSS and reaction by-products by the addition of 0.5 ml of w-butanol. Mix vigorously by vortexing and centrifuge (1 min, 15,000 rpm) to separate the two phases. Carefully remove the upper layer and discard. Extract two more times with w-butanol. 

To extract excess reactant, add to the reaction medium, 3 ml of w-butanol and 3 ml of water. Mix well. Centrifuge the mixture to separate the two phases. Discard the upper yellow layer. Repeat the extraction process several times, then dry the remaining solution containing activated oligo using a lyophilizer or a rotary evaporator. The PDITC-activated DNA is stable in a dry state. 

Aniline phthalate An aniline (1 g)/o-phthahc acid (1.5 g) in w-butanol (100 ml) (saturated with water) is sprayed on the plate, which is then heated at 105°C (10 min), yielding a variety of colors. 

Rump [17] has described a cellulose thin layer method for the detection of phenolic acids such as iw-hydroxybenzoic acid, iw-hydroxyphenylacetic acid and m-hydroxyphenylpropionic acid, in water samples suspected to be contaminated with liquid manure. The phenolic acid is extracted with ethyl acetate from a volume of acidified sample equalling lmg of oxygen consumed (measured with potassium permanganate). The ethyl acetate is evaporated and the residue dissolved in ethanol. After spotting of a lpm aliquot on a cellulose plate the chromatogram is developed by capillary ascent with the solvent n-propanol-w-butanol-25% NH3-water (4 4 1 1 by vol). The solvent front is allowed to advance 10cm. The air-dried plate is sprayed with a diazotised p-nitroanilinc reagent to make the phenolic acids visible. 

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