The reaction results in the production of somewhat complex mixtures of alkylene amines, including cyclic condensation products such as piperazines. 1100 ml) is decanted. I. Benzyl Esters from Methyl Esters and Benzyldimethylamine. For comparison, a reference oil is used containing a commercially available succinimide prepared from tetraethylene pentamine (TEPA) and a polyisobutenylsuccinic anhydride (PIBSA) having a nitrogen content of 2.1%. 25.1 g of the sulfonate used in Example B and 7.5 g (2.9 equivalent ratio) of di-n-hexylamine are reacted at 180° C. (reflux) for 22 hours. Subsequent to the reaction, the adduct can be purified by conventional techniques such as extraction with a lower alkanol (e.g., methanol), followed by vacuum distillation to remove light ends from the product. The lower layer is then discarded and the upper layer filtered through Celite 512 and then stripped using a rotary evaporator to yield 1610 g of polyisobutenylsulfonyl chloride. At the end of the 7-hour reaction period, the remainder of the reaction mixture (569 g) is transferred to a 2-liter, three-neck flask using about 50 ml of the hydrocarbon thinner to rinse the reaction flask. In the test on the lubricating oil compositions of this invention, the 1-G test is run for 60 hours. Before this distillation operation, it is often desirable to sparge the reaction product with an inert gas such as nitrogen at elevated temperatures, e.g., about 150° C. to about 200° C., generally for several hours, e.g., 1 to 8 hours, to reduce the amounts of entrained aromatic hydroxy compound and excess amine in the reaction product. 9.87 kg (10.39 g-mols) of a polybutene having a number average molecular weight of 950 is charged to the kettle under a nitrogen blanket. In an alternative preparation of the hydrocarbylsulfonic acid, the hydrocarbon is first reacted with an alkyl chlorosulfonate, optionally in the presence of a solvent such as 1,2-dichloroethane, ether, and the like. Such polar substituents are exemplified by chloro, keto, alkyloxy, etc. (b) To 14.6 g of the polyisobutenylsulfonyl chloride prepared in (a) above is added 60 ml pentane and 0.6 g tetraethylene pentamine. 18 publications. Noncomplexing solvents such as a mineral oil or a nonreactive organic solvent such as heptane, hexane, nitrobenzene, dichloroethane or various dichlorobenzenes may be used in addition to the complexing diluent. 8.2 Resuspend the pellet from ethanol precipitation in 200 μL of 50% formamide, and incubate at 55°C for 5 minutes to disrupt any secondary structure. The solution is filtered through diatomaceous earth and placed in a 3-liter, three-neck flask. continuation-in-part of U.S. application Ser. This procedure yields a metal salt of the hydrocarbylsulfonic acid ester, for example, sodium hydrocarbylsulfonate. b. Chemical approaches for detection and destruction of nerve agents. Polymerization of ε-Caprolactone Using Bis(phenoxy)-amine Aluminum Complex: Deactivation by Lactide. Both primary and secondary amines can be utilized. The supernatart hexane layer is decanted from some sludge-like material and is washed once with water, then filtered through Celite 512 and stripped using rotary evaporation. Brasch, U.S. Pat No. Suitable diluents for the concentrate include any inert diluent. 4.3 Centrifuge the solution in a microcentrifuge at ~12,000 × g for 30 minutes. One such internal combustion engine test is the severe Ford V-8 piston varnish test. ETHANOL PRECIPITATING THE LABELED OLIGONUCLEOTIDE Following the reaction, the labeling mixture contains labeled oligonucleotide, unlabeled oligonucleotide, and unincorporated dye (or biotin or DNP). 25.0 g of the sulfonate used in Example H and 12.0 g (9.9 mol ratio) of dimethylaminopropylamine are reacted at 125° C. (reflux) for 2 hours. The hydrocarbylsulfonic acid or salt prepared by either of the above procedures is then treated with a Vilsmeyer-Haack reagent, that is, an essentially 1:1 complex of a di-C1 -C4 alkyl formamide such a dimethyl formamide and an inorganic chloride such as phosphorus cxychloride or thionyl chloride and the like to form the corresponding hydrocarbylsulfonyl chloride. Nuha … 4 μL of a 25 μg/μL oligonucleotide stock solution (step 4.5). Search 512 g (0.357 mol) of a polyisobutenyl chloride (4%w chlorine prepared from a polyisobutene having a number average molecular weight of 1400), and 97 g (0.43 mol) o-chlorophenyl vinylsulfonate are charged to the flask. For oligonucleotides labeled with very hydrophobic dyes, like Texas Red® dye, you can achieve good separation running a faster gradient with up to a 3% increase per minute. You can purify the labeled oligonucleotide from the reaction mixture using preparative gel electrophoresis or reverse-phase HPLC. Analysis: S, 0.62%w; N, 1.79%w. 600 ml of n-hexane is added to the flask and the mixture is stirred for 2 minutes. 800 ml) is decanted. Analysis: Cl, 0.024%w; S, 1.06%w; N, 0.57%w. For much smaller or larger proteins, select a gel filtration media with a suitable molecular weight cutoff, or purify the conjugate by extensive dialysis (see step 2.1 below). 25.0 g of the sulfonate used in Example B and 5.4 g (4.5 equivalent ratio) of morpholine are reacted at 150° C. for 28 hours. In the above formulas I and II, Aryl represents an aryl radical or a substituted aryl radical. In this test, a Ford V-8 engine of 302-inch3 displacement is cycled through idle/cold/hot cycles at an RPM of 500/2500/2500 at water temperatures of 115/125/170° F., and a gallery temperature of 120/170/205° F. for periods of 45/120/75 minutes, respectively. The reaction mass is heated with stirring at 210° C. for 7 hours while maintaining a nitrogen atmosphere in the flask. 1 Average of 2 tests 2 Average of 8 tests. Analysis: 14.8-15.4% S. Adduction of o-chlorophenyl vinylsulfonate to polybutene. Reaction Buffer Amine-reactive reagents react with the non-protonated amine group on the modified oligonucleotide. Hydroxylamine may also remove dye from unstable conjugates with tyrosine, serine, threonine and histidine. This article is cited by Periodically throughout the reaction, the pH of the reaction mass in the 5-liter flask is checked. Using the same apparatus and the same procedure, phenyl vinylsulfonate is prepared from a charge of 253 g of phenol in the 5-liter reaction flask. Agitation is stopped and phase separation is allowed to take place. Analysis: Cl, 0.12%wt; S, 1.14%w; N, 0.89%w. Place the vial on a shaker oscillating at low speed, gently vortex to mix, or tap the vial every half hour for the first two hours to ensure that the reaction remains well mixed. 25.0 g of the sulfonate used in Example B and 14.0 g (7.9 equivalent ratio) of di-n-butylamine are reacted at 170° C. (reflux) for 4 hours. In a first embodiment the sulfonamide compositions are obtained by reacting: (a) the aryl ester of the substantially saturated hydrocarbylethylsulfonic acid or (b) a substantially saturated hydrocarbylsulfonyl chloride with a nitrogen-containing compound containing at least one amine hydrogen, i.e., --NH function. (a) To a 3-liter reaction flask is charged 750 ml of chlorosulfonic acid. A 500-ml, four-neck flask is fitted with a bottom outlet. the Altmetric Attention Score and how the score is calculated. if you were to add acid to the ester reaction would it react faster???? Hydrogenation of Alkenes with NaBH4, CH3CO2H, Pd/C in the Presence of O- and N-Benzyl Functions. The reaction mixture is stirred while 209 g of dimethyl formamide is added, followed by the dropwise addition of 189 ml of thionyl chloride while the temperature is maintained below 30° C. The reaction mixture is stirred for 2 hours at room temperature and then diluted wtih 400 ml hexane and allowed to stand for 4 hours.
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