Separatory funnel Teflon

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). 

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). 

The following procedure describes the preparation and analysis of the (R)-a-methylbenzylamide of (R)-a-methylbenzenepropanoic add. A flame-dried, 10-mL, round-bottomed flask equipped with a Teflon-coated magnetic stirring bar and a rubber septum is charged with 25 mg (0.15 mmol) of (R)-a-methylbenzenepropanoic acid, 31 mg (0.23 mmol) of 1-hydroxybenzotriazole hydrate, 44 mg (0.23 mmol) of 1-(3-dimethylamino)propyl-3-ethylcarbodiimide hydrochloride, and 0.50 mL of anhydrous N,N-dimethylformamide. This mixture is stirred at 23°C for 10 min, then cooled to 0°C in an ice-water bath. To the cooled solution, 24 pL (0.19 mmol) of R-(+)-a-methylbenzylamine and 86 pL (0.62 mmol) of triethylamine are added. Within 1 min, a fine white precipitate appears. The mixture is stirred for 1 hr at 0°C, then warmed to 23°C. After stirring for 20 hr at 23°C, the mixture is transferred to a 30-mL separatory funnel with 10 mL of dichloromethane. The product solution is extracted, sequentially, with four 10-mL portions of 1 N aqueous hydrochloric acid solution, 10 mL of saturated... 

The Teflon bed was eluted with 4 bed volumes of methylene chloride, which was collected directly into a separatory funnel. The water layer that formed in the eluate was separated and discarded. This methylene chloride became par fait fraction 1 (FI). 

The reaction mixture foams somewhat and acquires a succession of colors. The flask is mounted in a pan of acetone, a mechanical stirrer with a curved Teflon blade is placed in the center neck of the flask and operated slowly, and a 250-ml. separatory funnel is mounted into a side neck. Three flasks are put in an ice bath to cool one containing 190 ml. of distilled water, another 230 ml. of 29% ammonium hydroxide, and another 400 ml. of methylene chloride. 

Camphorsultam. A dry, 2-L, three-necked, round-bottomed flask is equipped with a 1.5-in egg-shaped Teflon stirring bar, a 250-mL addition funnel, and a 300-mL Soxhlet extraction apparatus equipped with a mineral oil bubbler connected to an inert gas source. The flask is charged with 600 mL of dry tetrahydrofuran (THF) (Note 1) and 6.2 g (0.16 mol) of lithium aluminum hydride (Note 2). Into the 50-mL Soxhlet extraction thimble is placed 35.0 g (0.16 mol) of (-)-(camphorsulfonyl)imine (Note 3) and the reaction mixture is stirred and heated at reflux. After all of the (camphorsulfonyl)imine has been siphoned into the reaction flask (3-4 hr), the mixture is allowed to cool to room temperature. The unreacted lithium aluminum hydride is cautiously hydrolyzed by dropwise addition of 200 mL of 1 N hydrochloric acid via the addition funnel (Note 4). After the hydrolysis is complete the contents of the flask are transferred to a 1-L separatory funnel, the lower, silver-colored aqueous layer is separated, and the upper layer placed in a 1-L Erlenmeyer flask. The aqueous phase... 

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... 

Teflon TFE (tetrafluoroethylene). This material is opaque and white and has the lowest coefficient of friction of any solid. It makes superior stopcock plugs and separatory funnel plugs. 

A 2-L, three-necked, round-bottomed flask equipped with a thermometer and a mechanical stirrer with Teflon blades is charged with a solution of the reaction product in 750 mL of ether. The contents of the flask are cooled in an ice-water bath to 3 C. To the flask 1s added a precooled (3°C) solution of 20 g (0.50 mol) of sodium hydroxide in 500 mL of brine (Note 11). The two-phase mixture is stirred vigorously for 1 hr with continued cooling (Note 12) and then Is transferred to a separatory funnel. The aqueous phase is separated and extracted with two 150-mL portions of ether (Notes 13, 14). The combined organic solution (Note 15) is dried over sodium sulfate and filtered. Solvent removal with a rotary evaporator at 35°C (70 mm) followed by concentration with the rotary evaporator at 35°C (12 nm) for 1.0 hr gives 24.7-25.0 g of crude (2S,3S)-3-propyloxiranemethanol as a pale amber oil (Note 16). 

A 0.5-ml portion of an internal solution (5 mg of bibenzyl/ml benzene) is added to the combined reaction solution and washings in the 80-ml beaker and filtered through a glass filter paper which subsequently is washed several times with ethyl ether. The combined filtrate and washings from this operation are transferred to a separatory funnel and a NaCI-saturated aqueous solution is added to deactivate the boron trifluoride. The funnel is shaken vigorously and the ether layer is removed and concentrated to about 10 ml by film evaporation. The concentrate is transferred to a glass vial fitted with a Teflon-lined cap and dried overnight over anhydrous sodium sulfate. 

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