Funnel , addition stopcock. Teflon

Modified Parfait Protocol. Teflon adsorbents were cleaned by 24-h extraction with acetone in a Soxhlet apparatus and stored in acetone. Cleaned Chromosorb T was used to fill a 150-mL silanized addition funnel equipped with a 24-40 male joint on the bottom. A plug of silanized glass wool supported the bed just above the stopcock. The Teflon bed was compressed slightly with a large stirring rod to keep the top of the bed in place while the bed was washed with at least 6 bed volumes (900 mL) of high-purity water. The washed Teflon was kept covered with water and used immediately. 

The Teflon and ion-exchange beds were eluted with the eluents as follows The addition funnels containing each bed were separated from the parfait column, and a separate, empty, addition funnel was loosely mounted on top to supply eluents. The bottom stopcock was closed, and the first eluent was slowly added until air escaped the bed and the bed was covered by 0.5 cm of liquid. The upper addition funnel was then firmly seated, and elution began by opening the bottom stopcock. Flow was adjusted to less than 3 mL/min with... 

A. 1-Diazo-4-phenyl-2-butanone. A 1-L Erlenmeyer flask equipped with a two-inch magnetic stirring bar and a two-hole rubber stopper fitted with a 125-mL Teflon stopcock separatory funnel (Note 2 and a drying tube filled with potassium hydroxide (Note 3) is charged with a solution of 200 mmol (3.4 equiv) of diazomethane (Note 4) in 600 mL of dry ether. The solution is cooled to 0°C and stirred at high speed (Note 5). To this cooled solution, 10.0 g (59 mmol) of hydrocinnamoyl chloride (3-phenylpropionyl chloride) (Note 6) diluted to 125 mL with anhydrous ether is added dropwise over a 1 -hr period. The resulting reaction mixture is stirred cold for an additional 0.5 hr and then at room temperature for 1 hr. After this period of time the... 

Fig. 1. Apparatus for the preparation of magnesium dihydride A, magnetic stirrer B, Teflon-coated stirring bar C, 250-ml, three-necked, round-bottomed flask D, water-cooled condenser E, pinch clamp F, 100-mL dropping funnel G, three-way stopcock H, stopcock to addition funnel I, mineral-oil bubbler J, Tygon tubing.

A 250-ml, three-necked, round-bottomed flask (to which is attached at the bottom a coarse-sintered-glass frit, a Teflon stopcock, and a standard-taper male joint) is equipped with a 100-ml pressure-equalizing addition funnel, a reflux condenser, and a Tru-bore glass mechanical stirrer with a Teflon blade. The system is flushed with dry nitrogen via a gas inlet in the addition funnel and a gas outlet in the condenser, leading to a mineral-oil bubbler. Magnesium turnings (3.5 g, 0.144 mole) and 100 ml of sodium-dried diethyl ether... 

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