Chromatographic reactor solution

In the scalar case (i.e., N = 1), wave solutions are easily constructed with the equilibrium diagram y(x) or Y(X). According to the above considerations, typical scalar problems are a binary nonreactive distillation process, a ternary reactive distillation process with a single chemical reaction, a reactive distillation process with Nc components and Nc - 2 chemical reactions, or a chromatographic reactor with Ns solutes... 

A solution of 500 mg 3 -acetoxypregn-5-en-20-one-[17a,16a-c]-A -pyrazoline in 100 ml of anhydrous dioxane is stirred with a magnetic stirrer and irradiated in a water-cooled quartz reactor with a high pressure Biosol Philips 250 W quartz lamp for 1 hr. The solvent is removed at reduced pressure and the residue is chromatographed on alumina (activity III). Elution with petroleum ether-benzene (3 1) gives 0.2 g (42%) of 3 -acetoxy-16a,17a-methylene-pregn-5-en-20-one mp 193-193.5° after two recrystallizations from methylene dichloride-ethyl acetate. 

A solution of the 2-azido ester or amide (ca. 2 g) in a mixture of MeOII (95 mL) and sodium-dried THF (95 mL) was photolyzed under N2 in a Hanovia photochemical reactor (110-W medium-pressure Hg lamp with a Pyrex filter). The reaction was monitored by observing the rate of disappearance of the absorption band (Nf) at 2140 cm 1 (irradiation times of 3-5 h were generally required). When the reaction was complete the solvent was removed in vacuo and the brown residual oil chromatographed on alumina [petroleum ether (bp 60-803C)/benzene 7 3]. Further elution with benzene followed by removal of the solvent gave the product (the esters as pale yellow oils, the amides as crystalline solids), which were further purified by vacuum distillation or by recrysiallization. 

A platinum on silica gel catalyst was prepared by impregnation of silica gel (BDH, for chromatographic adsorption) by a solution containing 0.5% (wt.) of sodium hydroxide and 0.5% (wt.) of chloroplatinic acid (both of analytical grade). The dried catalyst contained 1% (wt.) of platinum and a corresponding amount of the alkaline component. The BET surface area of the catalyst was 40 m2/g, the mean pore radius 150 A. The catalyst was always reduced directly in the reactor in a stream of hydrogen at 200°C for 2 hr. 

Fig. 1. Continuous-flow-apparatus for the optimization of homogeneous catalytic processes. A, catalyst solution B, starting compounds C, thermostated reactor D, trap E, gas-chromatograph F, data evaluation.

A fluorometric method was developed for determination of atmospheric H2O2 simultaneously with other species present at ppbv or lower levels, avoiding chromatographic separation. H2O2 is selectively collected by diffusion through a Nafion membrane, and is carried by a water stream into a reactor where it oxidizes thiamine hydrochloride (117) to a fluorescent ionic form of thiochrome (118), catalyzed by bovine hematin (75b) in alkaline solution, as shown in equation 40. The end solution containing 118 is passed through... 

Reductive alkylation is an efficient method to synthesize secondary amines from primary amines. The aim of this study is to optimize sulfur-promoted platinum catalysts for the reductive alkylation of p-aminodiphenylamine (ADPA) with methyl isobutyl ketone (MIBK) to improve the productivity of N-(l,3-dimethylbutyl)-N-phenyl-p-phenylenediamine (6-PPD). In this study, we focus on Pt loading, the amount of sulfur, and the pH as the variables. The reaction was conducted in the liquid phase under kinetically limited conditions in a continuously stirred tank reactor at a constant hydrogen pressure. Use of the two-factorial design minimized the number of experiments needed to arrive at the optimal solution. The activity and selectivity of the reaction was followed using the hydrogen-uptake and chromatographic analysis of products. The most optimal catalyst was identified to be l%Pt-0.1%S/C prepared at a pH of 6. 

V. Balakotaiah s treatment of Dispersion in Chemical Solutes in Chromatographs and Reactors 4 Carr s Applications of Center Manifold Theory5 is the standard text. 

Crystals were spread over a strip of Parafilm . Both the photochemical reactor and the strip with crystals were placed in a dry box and purged with nitrogen for 1 h. A 40 mg portion of 4-methyl-6,6-diphenylbicyclo[3.1.0]hex-3-en-2-one 1 was irradiated under conditions described above for 10 min through a 5 mm filter solution of 10 3 M sodium metavanadate in 5% sodium hydroxide. The mixture was chromatographed on preparative TLC plate eluted with 7% ether in hexane. Band 1 (28.0 mg, 70%) contained 3-methyl-4,5-diphenylphenol 2. Crystallization from hexane gave 14.1 mg (35%) of colorless crystals, mp 109-110 °C. 

To a benzene (40 ml) solution of alcohol (0.4 mmol) in a stainless reactor of autoclave was added Pb(OAc)4 (295 mg, 0.6 mmol). The inside of the reactor was flashed twice with 10 atm of carbon monoxide. Then the reactor was pressured at 80 atm with carbon monoxide and heated at 40 °C with stirring for 3 days. After the reaction, the mixture was poured into 0.4 M aq. HC1 solution, and extracted with ether thrice (20 ml X 3). The organic layer was dried over Na2S04 and filtered. After removal of the solvent, the residue was chromatographed on silica gel (eluent ethyl acetate/hexane = 1/9) to obtain 8-lactone in 51% yield [144]. 

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