Equipment overhead stirrer

A. 9-Phenyl-9-fluorenol. A flame-dried, 3-L, three-necked, round-bottomed flask equipped with an overhead stirrer, rubber septum, and glass stopper, under a nitrogen atmosphere, is charged with bromobenzene (158 mL, 1.5 mol, Note 2) and ethyl ether (800 mL, Note 2). The solution is cooled in an ice bath and stirred at 0°C. 

To 11.Og (12.3 mmol) of Wang resin (Note 1) in an oven-dried, solid-phase reaction flask (Note 2) equipped with an overhead stirrer and a nitrogen line attached to a bubbler was added 100 mL dichloromethane. The resultant slurry was allowed to stir for... 

C. (R,R)-N,N -Bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediamine. A 2-L, three-necked, round-bottomed flask equipped with a mechanical overhead stirrer, reflux condenser, and an addition funnel is charged with 29.7 g of (R,R)-1,2-diammoniumcyclohexane mono-(+)-tartrate salt (0.112 mol), 31.2 g of potassium carbonate (0.225 mol, 2 eq), and 150 mL of water. The mixture is stirred until dissolution is achieved, and 600 mL of ethanol is added. The cloudy mixture is heated to reflux with a heating mantle and a solution of 53.7 g (0.229 mol, 2.0 eq) of 3,5-di-tert-butylsalicylaldehyde in 250 mL of ethanol is then added in a slow stream over 30 min (Note 19). The addition funnel is rinsed with 50 mL of ethanol and the mixture is stirred at reflux for 2 hr before heating is discontinued. Water, 150 mL, is added and the stirred mixture is cooled to <5°C over 2 hr and maintained at that temperature for another hour. The yellow solid is collected by vacuum filtration and washed with 100 mL of ethanol. After the solid is air dried, it is dissolved in 500 mL of methylene chloride. The organic solution is washed with 2 x 300 mL of water, followed by 300 mL of saturated aqueous sodium chloride. The organic layer is dried over sodium sulfate, and filtered to remove the drying agent. The solvent is removed by rotary evaporation to yield the product as a yellow solid, mp 200-203°C (Notes 20 and 21). 

O. (R,R)-N,N -Bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediamino manga-nese(lll) chloride. A 2-L, three-necked, round-bottomed flask equipped with a mechanical overhead stirrer, reflux condenser, and a 500-mL addition funnel is charged with 67.2 g (0.27 mol 3 eq) of manganese acetate tetrahydrate (Mn(0Ac)2-4H20) and 500 mL of ethanol. Stirring is begun and the solution is heated... 

A. Preparation of an ether solution of phenylmagnesium bromide (Note 1). Ether (100 mL) is added to magnesium (Mg) turnings (74.6 g, 3.07 mol) in a dry, S-L flask equipped with an overhead stirrer, reflux condenser, and addition funnel. Iodine (several crystals) is added and the mixture is stirred for several minutes (the color dissipates). Bromobenzene (9.23 mL, 13.76 g, 87.64 mmol) is added and the mixture is heated with a heat gun to initiate the reaction. A solution of bromobenzene (322.8 mL, 481 g, 3.06 mol) in ether (600 mL) is added dropwise over 2.75 hr, maintaining a gentle reflux. The dark brown mixture is stirred an additional 3 hr at ambient temperature under nitrogen and then cooled in an ice/methanol bath to 0°C. 

B. N,N-Diethyl-2-formyl-6-methoxybenzamide (3). An oven-dried, threenecked, 1-L flask equipped with a 100-mL pressure equalizing dropping funnel, nitrogen bubbler, internal low temperature thermometer pocket, and overhead stirrer is flamed under reduced pressure and allowed to cool under a stream of nitrogen. The flask is charged with 500 mL of THF (Note 6) and cooled to an internal temperature of -72°C. N,N,N, N -Tetramethylethylenediamine (TMEDA) (Note 8) (23.5 mL, 0.156 mol) followed by 128.7 mL (0.157 mmol) of 1.22 M sec-butyllithium in cyclohexane (Note 9) are then added. The internal temperature rises a little as the reagents are added. The fluorescent yellow solution is allowed to recool to an Internal temperature of -73°C. 

B. Fluoromethyl phenyl sulfone (2). To a 3-L, three-necked, round-bottomed flask, equipped with an overhead stirrer, thermometer, and 1-L addition funnel with sidearm are added Oxone (221.0 g, 0.36 mol) (Note 9) and water (700 mL). The mixture is cooled to 5°C and a solution of the crude fluoromethyl phenyl sulfide (1) in methanol (700 mL) is placed in the addition funnel and added in a slow stream to the stirring slurry. After addition of the sulfide, the reaction mixture is stirred at room temperature for 4 hr, (Note 10) and the methanol is removed on a rotary evaporator at 40°C. The remaining solution is extracted with methylene chloride (2 x 500 mL). The combined organic layers are dried over magnesium sulfate, concentrated to ca. 150 mL, filtered through a plug of silica gel (230-400 mesh, 300 mL, 10 x 6.5 cm), and washed with an additional 500 mL of methylene chloride (Note 11). The colorless filtrate is concentrated and the resulting oil or solid is dried under vacuum (0.1 mm) at room temperature to provide 29 g of crude fluoromethyl phenyl sulfone (2) as a solid... 

Poly(triethynylbenzene) (PTEB, IV). highly capped. A 5-liter, 4-necked flask equipped with overhead stirrer, internal thermocouple, addition funnel, condenser, and heating mantle was... 

Type I Urea-Urethane Oligomers. To 30g (0.5 mole) ethylene diamine and lOg dimethoxy ethane in a three-neck flask equipped with an overhead stirrer was added over a one-hour period, 185g (0.5 mole) of butanol half-blocked dllsocyanate. After the addition, the reaction was stirred overnight at room temperature. 

Semicontinuous polymerization experiments were carried out in a stainless steel enclosure (dry box) under a dry nitrogen atmosphere in three neck flasks (11) equipped with overhead stirrer and an inlet for the continuous introduction of precooled inifer/isobutylene/ solvent feeds to stirred, dilute BCI3/solvent charges. Experiments with binifer were performed at -80°C by the use of CH3Cl/n-hexane solvent mixtures (80/20 v/v), with trinifer at -40°C using CH3CI... 

Under N2( >, 11.0 g (0.46 mol) of NaH and 400 mL of DME are added to a three-necked, 1-L, round-bottomed flask. The flask is equipped with a reflux condenser, an overhead stirrer, and an addition funnel charged with 15.7 g (0.157 mol) of pinacolone and 44.6 g (0.343 mol) of ethyl pivalate diluted with 30 mL of DME. The flask is heated at reflux and the contents of the addition... 

In a flask equipped with an overhead stirrer, a nitrogen inlet, and reflux condenser was placed 840 ml of dry THF and 20.0 g of 170-carboxylate 170-carbomethoxy ester of 4-aza-5a-androst-l-en-3-one (synthesized according to... 

As shown in Figure 1, a dry, 1-L, three-necked flask is equipped with an overhead stirrer bearing a four-bladed propeller of ca. 2.5-cm diameter... 

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