Funnel Teflon

Teflon stir bar 1 heavy duty balloon 1 roll of electrical tape Magnetic stirrer Support stand and clamps Ohaus triple beam scale 1 plastic funnel... 

The apparatus consists of a 1-1. three-necked flask equipped with a condenser, a dropping funnel, and a stirrer terminating in a stiff, crescent-shaped Teflon polytetrafluoroethylene paddle. The stirrer motor must have good torque (Note 1). The assembled apparatus, which is protected from moisture by means of drying tubes in the condenser and funnel, is preferably predried. About 216-224 g. (1.62-1.68 moles) of powdered anhydrous aluminum chloride is added to the apparatus with as little exposure to the moisture of the air as possible (Note 2). While... 

The reflux condenser was connected by an adaptor and Teflon tube to a trap of known weight which was cooled by a mixture of acetone and solid carbon dioxide. The flow of nitrogen was stopped, and an excess of water (about 15 ml.) was added dropwise through the dropping funnel to the stirred reaction product. The resulting mixture was heated at the reflux temperature, and the butane was collected in the trap. The weight of butane, b.p. —1° to 0°, was 4.23 1.35 g. (73-76% yield). 

Because of difficulties in adjusting an ordinary glass stopcock to avoid leakage and to maintain a drop rate that would add the un-saturated cyanoester solution over a 40-hour period, the checkers recommend the use of a funnel equipped with a Teflon stopcock. 

A. (E)-l-Propenyllithium. A dry (Note 2), 500-ml., three-necked, round-bottomed flask equipped with a Teflon -covered magnetic stirring bar, a 200-ml. pressure-equalizing dropping funnel, an efficient reflux condenser, and an immersion thermometer is capped with serum stoppers (Note 3) and flushed with argon (Note 4). Lithium dispersion (Note 5), [22.4 g. of a 50% wjw suspension in Amseo,... 

B. 4-Nonylbenzoic acid. A 500-mL, round-bottomed flask equipped with a Teflon-coated magnetic stirbar and a reflux condenser is charged with 4-nonylbenzoic acid methyl ester (10.07 g, 38.37 mmol), 100 mL of methanol (Note 1), and 96 mL of 1M aqueous NaOH. The resulting mixture is heated at reflux for 18 hr and then allowed to cool to room temperature. The reaction mixture is carefully acidified by addition of 200 mL of 1M aqueous HC1, and the resulting solution is transferred to a separatory funnel and extracted with four 250-mL portions of ethyl acetate. The combined organic layers are dried over Na2S04, filtered, and concentrated by rotary evaporation at reduced pressure. The residue (ca. 9.5 g) is recrystallized from 70 mL of hexanes to give 8.32-8.35 g (87-88%) of 4-nonylbenzoic acid as a white solid (Notes 6, 7). 

The importance of the linear arrangement of mixer/funnel/tubular reactor is shown when processing in a set-up with a curved flow element (0.3 m long bent Teflon tube of 0.3 mm inner diameter) in between the funnel and tubular reactor [78]. If a straight tube of equal dimensions as given above is used, plugging occius after 30 s. Hence even short curved flow passages are detrimental for micro-chan-nel-based amidation studies. 

A hydrolysis unit is constructed using the commercially available glassware shown in Figure 2. The collection funnel should be calibrated and marked for volumes of 35 and 85 mL. All 20/40-glass joints of the hydrolysis unit should be assembled with Teflon sleeves and secured with spring clamps to prevent loss of the volatile EMA and HEMA analytes. 

An attempt to place the wrong size or taper Teflon stopcock into the funnel. This is extremely rare. Get a new funnel. 

Two graduated dropping funnels of 500-ml. capacity equipped with pressure-equalizing tubes and small diameter tips to allow two solutions to be added in fine streams were used. They were also equipped with screw-in type plungers with Teflon fluorocarbon tips to allow fine adjustment of the flow rates. The checkers utilized standard 500-ml. dropping funnels and two needle valve adapters shown in Figure 1. 

A. 2-lodo-2-cyclohexen-1-one. A 500-mL, three-necked, round-bottomed flask equipped with a 1.5-in. Teflon-coated magnetic stirring bar, glass stopper, 50-mL addition funnel, and a reflux condenser is charged with a 1 1 mixture of 75 mL of anhydrous diethyl ether (Note 1) and 75 mL of pyridine. With vigorous stirring, 53 g (0.21 mol) of iodine (Note 2) is added slowly. At the completion of the addition, the dark brown mixture is stirred an additional 10-20 min until complete dissolution is obtained. 

C. 4a(S),8a(R)-2-Benzoyl-1,3,4,4a,5,8a-hexahydro-6(2H)-isoquinolinone (3). A 1-L, three-necked, round-bottomed flask is equipped with a mechanical stirrer, Teflon-coated thermocouple, 500-mL addition funnel and a N2 inlet. Concentrated sulfuric... 

A. (Z)-2,3-Dibromo-2-propenoic acid ethyl ester.2 Ethyl propiolate (9.01 g.91.8 mmol) and carbon tetrachloride (75 mL) are added in sequence to a 250-mL, round-bottomed flask equipped with a Teflon-coated magnetic stirring bar (Note 1). The flask is fitted with a 30-mL pressure equalizing addition funnel to which elemental bromine... 

A dropping funnel with a needle valve, NORMAG type 8056, manufactured by NORMAG GmbH, D-6238 Hofheim, FRG, has been used by the submitters. The checkers used a standard pressure-equalizing dropping funnel with a Teflon stopcock. 

To the flask are added 13.4 g. (0.58 mole) of clean sodium and 200 ml. of absolute toluene. The Vibromischer stirrer is activated, the toluene heated to reflux, and the agitation continued at this temperature until all the sodium is pulverized into a very fine sand. The agitation is ceased, and the solution is allowed to cool to room temperature. The nitrogen flow rate is increased, the Vibromischer stirrer is replaced with a conventional sealed mechanical stirrer with a Teflon blade, and a solution of 85 g. (0.6 mole) of 2-carbomethoxycyclopentanone (Note 2) in 450 ml. of absolute benzene is placed in the addition funnel. 

In a 3-1., three-necked, round-bottomed flask fitted with a powerful slow-speed stirrer having a Teflon blade, a 500-ml. dropping funnel, and a thermometer arranged to dip into the liquid is placed 588 g. (366 ml., 6 moles) of concentrated sulfuric acid. The flask is surrounded by an ice-salt mixture, the stirrer started, and 1216 g. (1170 ml., 12 moles) of acetic anhydride (Note 1) is added at such a rate that the temperature does not rise above 20° (Note 2). The separatory funnel is removed and 912 g. (6 moles) of coarsely powdered D,L-camphor is added (Note 3). The flask is then closed with a stopper and stirring is continued until the camphor is dissolved. The stirrer is replaced by a stopper, the ice bath allowed to melt, and the mixture left to stand for 36 hours (Note 4). The camphorsulfonic acid is collected on a suction filter and washed with ether (Note 5). After being dried in a vacuum desiccator at room temperature, the nearly white crystalline product weighs 530-580 g. (38-42%). It melts at 202-203° with rapid decomposition and is relatively pure (Note 6). 

In a dry 3-1. three-necked round-bottomed flask, equipped u il.h a sealed mechanical stirrer (all-glass or glass-Teflon), a l ( llux condenser fitted with a calcium chloride drying tube and a 100-ml. dropping funnel, are placed 50.0 g. (0.500 mole) of (inely powdered succinic anhydride (Note 2), 133.4 g. (1.00 mole) of freshly crushed anhydrous aluminum chloride (Note 3), and 500 ml. of anhydrous 1,2-dichloroethane. The mixture is Hl.irred vigorously at room temperature for about 2 hours to dissolve as much as possible of the solid reactants. Then 50.0 g. (0.500 mole) of isopropimyl a< [Pg.81]

A 2-1. fouir-necked flask equipped with a sealed, Teflon-paddle stirrer, a merrcury thermometer, a gas inlet tube, and a dropping funnel is charged with 1.21. of anhydrous tetrahydrofuran (Note 1) and 50 g. (7.1-g. atoms) of lithium pieces (Note 2) under an atmosphere of prepurified nitrogen. The stirred mixture is cooled to —20° by means of a dry ice-acetone bath and a mixture of 100 g. (1.00 mole) of methyl methacrylate (Note 3), and 411 g. (3.0 moles) f n-butyl bromide (Note 4) is added dropwise over a period off 3-4 hours. During this addition, an exothermic reaction ensues which is controlled at —20° (Note 5), and on completion of the addition, the vessel is maintained at this temperature, with stirring, for an additional 30 minutes. The contents oF the flask are then liltered with suction through a... 

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