Mmol

The adsorption of the surfactant Aerosol OT onto Vulcan Rubber obeys the Langmuir equation [237] the plot of C/x versus C is linear. For C = 0.5 mmol/1, C/x is 100 mol/g, and the line goes essentially through the origin. Calculate the saturation adsorption in micromoles per gram. 

To a stirred solution of 0.5 ml of 10% aqueous sodium hydroxide and 8.25 mmol of the appropriate aldehyde in 10 ml of ethanol, 8.25 mmol of 2-ace tylpyri dine was added drop wise during 2-3 hours. The temperature was kept at 0°C. After stirring for another 2 hours the reaction mixture was filtered, yielding almost pure solid 2.4a (7.26 mmol, 88%) or 2.4b (7.76 mmol, 94 %). After crystallisation... 

A suspension of 3.90 g (19.6 mmol) of p-(bromomethyl)benzaldehyde (2.8) and 4.00 g (31.7 mmol) of sodium sulfite in 40 ml of water was refluxed for two hours, after which a clear solution was obtained. The reaction mixture was cooled on an ice bath resulting in precipitation of some sodium sulfite. After filtration, the solvent was evaporated. Ethanol was added to the remaining solid and the suspension was refluxed for 10 minutes. After filtering the hot solution, the filtrate was allowed to cool down slowly to -18 °C whereupon sodium (p-oxomethylphenyl)methylsulfonate (2.9) separated as colourless crystals. The extraction procedure was repeated two more times, affording 2.29 g (10.3 mmol, 53%) of the desired product. H-NMR (200 MH D2O) 5(ppm) =4.10 (s,2H) 7.44 (d,2H) 7,76 (d,2H) 9.75 (s,lH). 

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. 

Endo-exo ratios of the micelle-catalysed reactions have been determined by adding 0.25 mmol of 5.1c and 0.5 mmol of 5.2 to a solution of 5 mmol of surfactant and 0.005 mmol of EDTA in 50 ml of water in carefully sealed 50 ml flasks. The solutions were stirred for 7 days at 26 C and subsequently freeze-dried. The SDS and CTAB containing reaction mixtures were stirred with 100 ml of ether. Filtration and evaporation of the ether afforded the crude product mixtures. Extraction of the Diels-Alder adducts from the freeze-dried reaction mixture containing C12E7 was performed by stirring with 50 ml of pentane. Cooling the solution to -18 C resulted in precipitation of the surfactant. Filtration and evaporation of the solvent afforded the adduct mixture. Endo-exo ratios... 

Synthesis of Alkviamines. General Procedures. Method (A). The synthesis of p-phenethylamine is representative. A flame dried, nitrogen-flushed, 100 ml flask, equipped with a septum inlet, magnetic stirring bar and reflux condenser ivas cooled to 0°C. Sodium borohydride (9.5 mmol, 0.36 g) was placed in the flask followed by sequential addition of THF (13-15 ml) and BF3-Et20 (12 mmol, 1.5 ml) at 0°C. After the addition, the ice bath was removed and the contents were stirred at room temperature for 15 min. The solution... 

Alkvl Azides from Alkyl Bromides and Sodium Azide General procedure for the synthesis of alkyl azides. In a typical experiment, benzyl bromide (360 mg, 2.1 mmol) in petroleum ether (3 mL) and sodium azide (180 mg, 2.76 mmol) in water (3 mL) are admixed in a round-bottomed flask. To this stirred solution, pillared clay (100 mg) is added and the reaction mixture is refluxed with constant stirring at 90-100 C until all the starting material is consumed, as obsen/ed by thin layer chromatographv using pure hexane as solvent. The reaction is quenched with water and the product extracted into ether. The ether extracts are washed with water and the organic layer dried over sodium sulfate. The removal of solvent under reduced pressure affords the pure alkyl azides as confirmed by the spectral analysis. ... 

In a 100ml three-necked, round-bottomed flask equipped with mechanical stirrer, thermometer and a reflux condenser, a vigorously stirred mixture of the above catalyst (0.7g, 0.31 mmol), safrole (13.24g, 80mmol), benzene (35 ml) and 40% w/v H2O2 (5.10ml, 60... 

Reaction with h (1.5 mmol) [or Br2], supported salt (1.5 mmol), alkene (0.625 mmol), in 5 ml of ethanol-free CHCia at room tem-... 

Direct Borohydride Reduction of Alcohols to Alkanes with Phosphonium Anhydride Activation N-Proovlbenzene. To a solution of 5.56 g (20 mmol) of triphenylphosphine oxide in 30mL of dry methylene chloride at CfC was added dropwise a solution of 1.57 mL (10 mmol) of triflic anhydride in 30mL of dry methylene chloride. After 15 min when the precipitate appeared, a solution of 1.36g (10 mmol) of 3-phenyl-1-propanol in 10 mL of dry methylene chloride was added and the precipitate vanished in 5 min. An amount of 1.5g (40 mmol) of sodium borohydride was added as a solid all at once and the slurry was stirred at room temperature for... 

MejSiCI - Nal - CH3CN as an Efficient and Practical Reducing Agent for Benzoic Alcohols. A typical procedure for the present reduction is as follows To a mixture of MejSiCI (1.54 ml, 12 mmol), Nal (1.8 g, 12 mmol), and acetonitrile (0.6 ml, 12 mmol) was added a solution of 1-phenylethanol (244 mg, 2 mmol) in hexane (2 ml). The mixture was stirred for 24 h at room temperature. Dilution with water, extraction with ether and subsequent isolation process gave ethylbenzene (158 mg) with sufficient purity in 75% yield. ... 

Synthesis by high-dilution techniques requires slow admixture of reagents ( 8-24 hrs) or very large volumes of solvents 100 1/mmol). Fast reactions can also be carried out in suitable flow cells (J.L. Dye, 1973). High dilution conditions have been used in the dilactam formation from l,8-diamino-3,6-dioxaoctane and 3,6-dioxaoctanedioyl dichloride in benzene. The amide groups were reduced with lithium aluminum hydride, and a second cyclization with the same dichloride was then carried out. The new bicyclic compound was reduced with diborane. This ligand envelops metal ions completely and is therefore called a cryptand (B. Dietrich, 1969). 

A mixture of 3-methoxy-2-nitro-P-pyrrolidinostyrene (lOg, 40 mmol) and Raney nickel (25 g) in methanol-THF (40 ml of each) was heated to 60"C and,... 

The o,p-dinitrostyrene (1 mmol) and ammonium formate (10 mmol) W ere dissolved in methanol and 10% Pd/ C (5% by wt) was added. The mixture was refluxed under nitrogen for 1 h. Formic acid (0.44 ml) w as added and reflux was continued for 0.5-1 h until the completion of the reaction (tic). The solution was filtered through Celite, evaporated in vacuo and eluted through silica gel with CH2CI2. 

Thionyl chloride (11.5g, 96.4 mmol) was added to 2-nitrophenylacetic acid (8.72g, 48.2mmol) and the suspension was warmed to 50°C and stirred until gas evolution was complete. The resulting solution was concentrated in vacuo and the residue dissolved in CHjClj (30 ml). This solution was added dropwise to a stirred solution of Meldrum s acid (6.94 g, 48.2 mmol) in CH2CI2 (200 ml) under nitrogen at 0 C. The solution was stirred at 0" C for 1 h after the addition was complete and then kept at room temperature for an additional hour. The reaction solution was then worked up by successively washing with dil. HC1, water and brine and dried (MgSOJ. The dried solution was concentrated in vacuo and abs. ethanol (200 ml) was added to the residue. The mixture was... 

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