Schlenk flask

A mixture of l,4-dibromo-2,5-bis(3-sulfonatopropoxy)benzene 61 (0.78 g, 1.39 mmol), 60 (0.23 g, 1.39 mmol), Na2C03 (0.99 g) in doubly distilled water (47 mL), and DMF (20 mL) was heated at 85°C until the solids were completely dissolved. The resulting solution was cannulated to a 200-mL Schlenk flask with tris[(sulfonatophenyl)phosphine]palladium(0) (0.045 g) and the mixture was stined at 85°C for 10 h. The reaction mixture was concentrated to 25 mL by boiling and filtered. The filtrate was added dropwise to cold acetone (250 mL) to precipitate out the polymer. The polymer was collected by filtration, redissolved in a minimum of hot water, and reprecipitated by cooling. After repeating this procedure twice, the polymer was redissolved in distilled water and dialyzed for 72 h in 3500 gmol 1 cutoff membrane. After drying under vacuum, polymer 63 was obtained in 64% (0.42 g). 

One 30 mL Schlenk flask equipped with magnetic stirrer bar... 

Once the clear reddish solution of the catalyst had cooled to room temperature, it was transferred under a gentle stream of nitrogen to a Schlenk flask containing a solution of the ketone (235 pL, 2 mmol) and potassium iso-propoxide (0.05 mmol, 2.5mol%) in z -PrOH (15 mL). The resulting solution was then stirred for 1.5 hours at room temperature under nitrogen (monitored by GC and/or 1 2 3 4H NMR). 

A 100 mL Schlenk flask equipped with a magnetic stirrer bar and a condenser was dried at 150 °C overnight, cooled under vacuum and then flushed with nitrogen. 

R, R. pS, p5)-l,l -bis [a-(Dimethylamino)propyl]-2,2 -bis(diphenylphosphi-no)ferrocene (1.55 g) and 4-dimethylaminopyridine were placed in a 25 mL degassed Schlenk flask equipped with a magnetic stirring bar acetic anhydride (4.00 mL) was then added. 

Silane redistribution 6 mg of (3-(methylsilyl)propyl) triphenylphosphonium hexafluorophosphate(V) (0.0121 mmol, 1 equivalent), 93 mg of Karstedt s catalyst (Pt 3.91% 0.000954 mmol, 0.8 equivalent), 6 mg of triphenylphosphine (0.0229 mmol, 1.9 equivalent) were dissolved in 20 mL of freshly distilled fluoroben-zene in a 50 mL Schlenk flask in an inert atmosphere glovebox. The flask was equipped with a septum, removed from the glovebox and installed with PEEK tubing leading to the mass spectrometer. The flask was pressurized with N2 and monitored by ESI-MS. Once a steady signal was obtained, 0.15 g of freshly distilled phenylsilane (1.39 mmol, 115 equivalents) was injected into the reaction flask. The reaction was initiated at room temperature and then was heated to reflux after 20 min to drive it to completion. 

Methoxy-2 -methylbiphenyl. o-Tolylboronic acid, 10.0 g (73.6 mmol) (Note 1), 16.8 g (71.8 mmol) of 4-iodoanisole (Note 2), and 200 mL of acetone (Note 3) are combined in a 1-L, three-necked flask equipped with an efficient stirbar, two stoppers, and a reflux condenser attached to a gas-flow adapter with a stopcock. Potassium carbonate, 25.0 g (0.180 mol), is dissolved in 200 mL of water (Note 4) in a separate 250-mL Schlenk flask. In a third flask (25-mL Schlenk flask) 3.30 mg (0.02 mmol, 0.2%) of palladium acetate (Note 5) is dissolved in 10 mL of acetone. All three flasks are then thoroughly degassed by four freeze-pump-thaw cycles. Under an argon back flow, one of the stoppers on the three-necked flask is replaced with a rubber septum, and the carbonate and catalyst solutions are added via cannula to form a biphasic mixture. The top layer turns brown upon addition of the catalyst. The septum is... 

Triphenylphosphine (100.3 g, 0.3825 mol) and copper(I) chloride (15.14 g, 0.1529 mol) were added to a dry, septum-capped 2 L Schlenk flask and placed under nitrogen. Benzene (distilled and deoxygenated, approximately... 

Care must be taken to avoid loss of product that is easily taken up in the syringe. The checkers found it more convenient to perform the reaction in a tared, round-bottomed Schlenk flask. Solvent was then removed from the solid dicyclohexylborane by filtration using a positive nitrogen flow. 

A mixture of 0.27 mtnol of tricyclo[3.3.1.1 3,7]decane (adamantane), 0.054 mmol of (Bu4N)4Wl()032, and 3 mg of platinum in 10 mL of acetonitrile under argon in a Pyrex Schlenk flask is irradiated with a 550 W mercury arc lamp. The reaction turns deep blue on photolysis. Every 16 h, photolysis is Stopped, the catalyst is reoxidized under air, the sample is degassed and again placed under an argon atmosphere, and irradiation is resumed. After a total of 64 h there is 58% conversion of adamantane and a 40% yield of the methyl ketone (by VPC). 

All compounds are routinely handled and stored under nitrogen in Schlenk flasks, although most solids can be handled safely in air. Solvents are dried and degassed before use. 

Chromium(III) chloride hexahydrate (30 g, 0.113 mol) is dissolved in 40 mL of distilled water and introduced to a Schlenk flask containing 40 g of zinc (20 mesh). The solution is carefully deoxygenated under vacuum and then saturated with argon. With the help of a cannula and a pressure gradient, 75 mL of deoxygenated hydrochloric acid (35%) is slowly added to the constantly stirred mixture. 

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