Morpholine VOLUME

The densities and volumetric specific heats of some alkali halides and tetraalkylammonium bromides were undertaken in mixed aqueous solutions at 25°C using a flow digital densimeter and a flow microcalorimeter. The organic cosolvents used were urea, p-dioxane, piperadine, morpholine, acetone, dime thy Isulf oxide, tert-butanol, and to a lesser extent acetamide, tetrahydropyran, and piperazine. The electrolyte concentration was kept at 0.1 m in all cases, while the cosolvent concentration was varied when possible up to 40 wt %. From the corresponding data in pure water, the volumes and heat capacities of transfer of the electrolytes from water to the mixed solvents were determined. The converse transfer functions of the nonelectrolyte (cosolvent) at 0.4m from water to the aqueous NaCl solutions were also determined. These transfer functions can be interpreted in terms of pair and higher order interactions between the electrolytes and the cosolvent. 

Figure 1. Electropherogram of hGH digest elution buffer, 0.1 M tricine, and 0.02 M morpholine, pH 8.15 injection volume about 9 nL.

Figure 5. Percent [Desamido-Asn-149] hGH vs. injection volume elution buffer, 0.01 M tricine, 0.0058 M morpholine, and 0.02 M NaCl, pH 8.0. Replicate values (points), average value (line), and standard deviation (error bars) as indicated.

When solutions of lactates are acidified with sulfuric acid, potassium permanganate TS (0.1 AO is added, and the mixture is heated, acetaldehyde is evolved. This can be detected by allowing the vapor to come into contact with a filter paper that has been moistened with a freshly prepared mixture of equal volumes of 20% aqueous morpholine and sodium nitroferricyanide TS. A blue color is produced. 

Acetaldehyde Test Paper Use a solution prepared by mixing equal volumes of a 20% solution of morpholine and a 5% solution of sodium nitroferricyanide. Saturate the prepared filter paper in the mixture, and use the moistened paper without drying. 

The Step 2 product (342.4 g) dissolved in 3400 ml EtOAc was treated with morpholine (85.80 g) dissolved in 340 ml EtOAc added over 90 minutes. The mixture was stirred 30 minutes, then treated with charcoal (35.2 g), and filtered through celite. Solids were washed with EtOAc, the filtrate volume reduced to 2000 ml, and 1700 ml heptane added. The suspension was stirred overnight, filtered, washed with the mother liquor, dried overnight, and the product isolated. 

A reactor was charged with (E)-N-butenyl morpholine (0.81 mmol), titanium tetrachloride 2THF (8 JLmol), di-isopropylethylamine (1.22 mmol), propionyl chloride (0.98 mmol), and 8.1 ml CH2CI2 and the mixture stirred until the allylic morpholine was consumed as determined by TLC. Thereafter, the mixture was diluted with an equal volume of diethyl ether, washed with aqueous 1 M NaOH, dried, and the product isolated by chromatography on silica gel using diethyl ether in 92% yield. H- and C-NMR and HRMS (FAB) data supplied. 

The high viscosity of concentrated sulfuric acid causes a fairly high backpressure, which was mandatory for residence times as short as possible. The homemade pilot plant continuous reaction system consisted of a static mixer and a residence time loop with a total volume of565 mb (Fig. 15.19). The maximum temperature of the whole system was limited to 60 °C, because it was foimd that the complete heat of reaction was liberated within one second during the flow through the static mixer. To control the reaction temperature in this scale correctly dimensioned heat sinks are mandatory. With these precautions the same results were obtained as before. Using this equipment over 200 kg of4-(phenyl)morpholin-3-one were nitrated within 50 h. 

Morpholine vapors form explosive mixtures with air within the range 1.8-11.0% by volume in air. 

Improved Isolation Procedure. Our improved method is based on ultrafiltration of the supernatant followed by purification of the crude enzyme on a carboxysulfone ion-exchange column. Treatment with DEAE cellulose, done after initial concentration of the supernatant, is optional but useful it removes about half of the concomitant proteins. In the final step, the crude solution is loaded in portions on the ion-exchange column and the void volumes are isocratically eluted after each injection with the 4-morpholine ethanesulfonic acid (MES) buffer. Finally, sodium acetate... 

Figure 4.57 Separation of alkali metals, alkaline-earth metals, and morpholine on lonPac CS12A. Eluent lOmmol/L H2SO4 (or 20mmol/L MSA) flow rate 1 mlVmin detection suppressed conductivity injection volume 25 pL ...

Fig. 9-53. Trace analysis of cations in presence of a large excess of ammonium and morpholine. -Separator column lonPac CS14 (2-mm) eluant 8 mmol/L methane-sulfonic acid - acetonitrile (95 5 v/v) flow rate 0.25 mL/min detection suppressed conductivity injection volume 1 mL pre-concentrated on lonPac CC14 (2-mm) solute concentrations 0.5 pg/L lithium (1), 2 pg/L sodium (2), 150pg/L ammonium (3),...

The reaction of NO with the double bonds of enamines also produces compounds containing the diazeniumdiolate functional group bound to carbon, and some of the compounds prepared in this way have the potential to serve as spontaneous NO donors [43]. The compounds chosen for study were enamines 1-4 derived from condensation of cyclopentanone or cyclohexanone with morpholine or pyrrolidine. When these enamines were dissolved in acetonitrile and treated with NO gas (5-atm pressure) at room temperature, a vigorous exothermic reaction resulted, accompanied by high uptake of NO and formation of a brown precipitate. Attempts to isolate the solid precipitates often resulted in rapid decomposition, with the release of large volumes of gaseous NO. At -78 °C in diethyl ether, the reaction of 4-(l-cyclohexen-l-yl) morpholine (IX) afforded a good yield of crystalline NO addition product (X) ... 

To prepare the [m-(acetylpyridinio)-n-alkyl]adenosine pyrophosphates, 10 mmoles of acetylpyridinio-n-alkylphosphoric acid and 10 mmoles of adenosine 5 -phosphoromorpholidate (as salt of 4-morpholine iV,iV -dicyclohexylcarboxamidine) are dissolved in 20 ml of freshly distilled o-chlorophenol. The mixture is stored at room temperature for 7 days. Progress of the condensation reaction is checked daily by paper electrophoresis (0.1 M Tris chloride at pH 8.1, 30 V/cm). After the reaction is completed, 60 ml of water are added to the mixture and the suspension is extracted 3 times, each with 200 ml of ethyl ether. The first ether extract obtained is reextracted with 30 ml of water. The combined aqueous phases are reduced to a volume of 5 ml under reduced pressure and are charged on to a Dowex 1X8 column (formate form, 2 X 50 cm, 100-200 mesh). The column is washed with 6.5 liters of water, and the coenzyme analogs are eluted from the resin with a convex gradient of formic acid ... 

Full details of the Ni - and Pd -catalysed telomerization reactions of butadiene with phenylhydrazones (see Volume 6, p. 388) have now been published. Reaction of butadiene with diethylamine gives (49 Z = NEta) in the presence of allyl M halides. The catalytic activity increases in the series M = Ni < M = Ptsimilar reactions of butadiene, especially virith cyclic secondary amines (e.g. morpholine). For M = Pd addition of AcOH improves the yield of (49 Z = NEta) whilst for M = Pt no telomers are formed in the absence of Al(OR)3 (R = Pr or Bu ) co-catalysts. The reaction of butadiene with acetic acid to give (49 Z = OAc) is also catalysed by [M(cod)2] although with the catalyst M = Pd l-vinylhex-5-enyl acetate is a by-product (20%). Reactions of butadiene with acetaldehyde and phenyl isocyanate in the presence of [Pd(cod)t]-2PPh3 give (50 and (51), respectively, ... 

The unmodified rhodium-catalyzed hydroaminomethylation of 1-octene and morpholine was investigated in ternary thermophoric solvent systems [26]. Therefore, hexane or dodecane, together with propylene carbonate and a mediator solvent, provided complete miscibility at the desired reaction temperature of 125 °C. N- and iso-N-nonylmorpholine products adopted the nonpolar phase after cooling and could be separated (Scheme 5.8). Applying a 1-octene/morpholine ratio of 1.5,96% amine selectivity was the highest achieved in the PC/dodecane/l,4-dioxane (1 0.55 1.3, volume ratio) polar/nonpolar/mediator solvent system. Rhodium loss was measured by ICP-OES to be less than 1.5% and was correlated to the mediator solvent polarity. 

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