Three-neck round-bottom flask

Apparatus 3-1 round-bottomed three-necked flask with a combination of dropping funnel and gas inlet tube, reaching 1 cm beneath the surface of the NH3, stirrer and a combination of thermometer and vent (see Chapter I, Fig. 1). 

Apparatus 200-ml round-bottomed, three-necked flask provided with a gas inlet, a thermometer and a gas outlet magnetic stirring. 

Apparatus 1-1 round-bottomed, three-necked flask, provided with a dropping funnel, a mechanical stirrer and a reflux condenser. 

Apparatus 1-1 round-bottomed, three-necked flask with a dropping funnel, a mechanical stirrer and a thermometer, combined with a vent, for the addition of bromine and the dehydrobromination to 1-bromocyclooctene 1-1 flask (see Fig. 1) for the preparation of cyclooctyne. 

Apparatus. 500-ml round-bottomed, three-necked flask with a gas inlet tube, thermometer and a gas outlet for the preparation of chlorotetrahydropyran 1-1 four--necked, round-bottomed flask with a gas inlet tube, a dropping funnel, a mechanical stirrer and a thermometer, combined with a gas outlet for the preparation of HC=CMgBr and its reaction with chlorotetrahydropyran 1-1 three-necked, round--bottomed flask with a dropping funnel, combined with a gas inlet, a mechanical Stirrer and a thermometer, combined with a gas outlet for the conversion into the allenic alcohol. 

Hove 1. The procedure described in Ref. 1 was modified. To a solution of 2.0 mol of lithium acetylide in 1.2 1 of liquid ammonia in a 4-1 round-bottomed, three-necked flask (see Fig. 2) was added 1.5 mol of freshly distilled benzaldehyde with cooling at about -45°C. After an additional 30 min finely powdered ammonium chloride (2 mol) was introduced in 15 min. The ammonia was allowed to evaporate, then water (1.1 1) was added and the product was extracted with diethyl ether. After drying over magnesium sulfate the extract was concentrated in a water-pump vacuum. High-vacuum distillation,... 

A MIXTURE of 120 g. (3 moles) of sodamide (Note i) and 200 cc. of purified mineral oil (Note 2) is ground together in a mortar until the amide is finely pulverized (Note 3). This suspension is transferred to a 2-I. round-bottom, three-necked flask fitted with a reflux condenser holding a calcium chloride tube, a 500-cc. separatory funnel, and an efficient mechanical stirrer through a mercury seal. The mortar and pestle are rinsed with an additional 250 cc. of the oil which is then added to the reaction flask. This is heated in an oil bath maintained at 160-165, the stirrer is started and 203 g. (i mole) of cyclohexylbromopropene (p. 20) is dropped in during one and one-half hours. Ammonia is evolved and this is allowed to pass through the condenser and is collected in water. 

A. Heptoic anhydride enanthic anhydride). In a 250-ml. round-bottomed three-necked flask, equipped with a stirrer, dropping funnel, and thermometer, are placed 15.8 g. (16.1 ml., 0.2 mole) of dry pyridine (Note 1) and 25 ml. of dry benzene (Note 2). I hen 14.8 g. (15.5 ml., 0.1 mole) of heptoyl chloride (Note 3) is added rapidly to the stirred solution. The temperature rises only slightly, and a pyridinium complex separates. While stirring is continued, 13.0 g. (14.1 ml., 0.1 mole) of heptoic acid (Note 3) is added from the dropping funnel over a period of 5 minutes. The temperature rises rapidly to 50-65° (Note 4), and pyridine hydrochloride is formed. After stirring for 10 minutes, the solid is collected on a chilled Buchner funnel and washed twice with 25-ml. portions of dry benzene (Note 5). 

A 3-1. round-bottomed three-necked flask is equipped with a mechanical stirrer, a 500-ml. dropping funnel, and a 250-ml. dropping funnel. The flask is contained in a pneumatic trough through which water at room temperature is circulated. A mix-... 

About half of the sodium ethylate solution is poured into a 3-]. round-bottomed, three-necked flask provided with a liquid-sealed stirrer and a reflux condenser the other half is kept warm by a small flame. The first half of the solution is allowed to... 

In a i-l. round-bottomed, three-necked flask fitted with an efficient reflux condenser, liquid-sealed stirrer, and dropping funnel is placed t3 g. (0.53 gram atom) of magnesium turnings. A few cubic centimeters of a solution of 60 g. (41.4 cc., 0.55 mole) of pure ethyl bromide in 50 cc. of absolute ether is added and the stirrer started (Note i). When the bromide begins to react 200 cc. of absolute ether is added, and then the balance of the bromide solution is run in as fast as the refluxing permits (about one-half hour). After allowing fifteen minutes for the completion of the reaction, a solution of 40 g. (0.42 mole) of 2,4-dimethyl-pyrrole (Org. Syn. 15, 20) in 100 cc. of absolute ether is added in the course of twenty minutes (Note 2) and the mixture is refluxed for one-half hour on the steam bath. 

In a 3-I. round-bottomed, three-necked flask fltted with a liquid-sealed mechanical stirrer, a thermometer, and a 500-cc. separatory funnel are placed 1700 cc. of dry ben2ene and 160 g. (1.2 moles) of powdered, anhydrous aluminum chloride (Note i). The mixture is cooled to 10° by means of an ice-water bath and maintained at 10-20 during the addition of a solution of 120 g. (0.58 mole) of benzalacetophenone (Note 2) (Org. Syn. Coll. Vol. I, 71) in 300 cc. of dry benzene. This addition requires about thirty minutes. The cooling bath is then removed and stirring continued at room temperature until all the dense, yellow precipitate formed at first has gone into solution (Note 3). The reaction is complete after stirring for an additional hour. 

A dry 500-ml round-bottomed three-necked flask fitted with a stirrer, internal thermometer, and a pressure-equalized dropping funnel is placed under nitrogen and the flask is charged with 0.148 mole of freshly distilled cyclohexanone and 0.148 mole of freshly distilled ethyl chloroacetate. A solution of 6.0 g of potassium and 125 mL of dry terr-butyl alcohol is introduced into the dropping funnel, and the system is exhausted and... 

In a 500-cc. round-bottomed, three-necked flask provided with a thermometer, dropping funnel, a liquid-sealed stirrer, and calcium chloride tube are placed 16.8 g. (0.2 mole) of thiophene (Org. Syn. 12, 72), 15.6 g. (0.2 mole) of acetyl chloride, and 200 cc. of dry benzene. The solution is cooled to o°, and 52 g. (23 cc., 0.2 mole) of freshly distilled stannic chloride is added dropwise, with efficient stirring, during the course of about forty minutes. The reaction mixture assumes a purple color when the first drops of stannic chloride are added, and soon a purple solid precipitates. 

A 5-1. round-bottomed three-necked flask is equipped with a Kyrides sealed stirrer (Org. Syn. 21, 40, Note 1) and two long condensers, and the apparatus is so arranged that, if necessary, the exit water from the condensers may be quickly used to cool the flask. 

In a 2-1. round-bottomed three-necked flask, fitted with an efficient reflux condenser, mechanical stirrer, and dropping funnel (Note 1), are placed 133.3 g. (1 mole) of anhydrous powdered aluminum chloride, 137.4 g. (1 mole) of phosphorus trichloride, and 184.6 g. (1.2 moles) of carbon tetrachloride (Note 2). The reactants are stirred slowly until they are thoroughly mixed, and then heat is applied carefully until the reaction begins. At this point the liquid boils vigorously, and the reaction mixture becomes thicker so that faster stirring is necessary. Finally, the stirrer is stopped when the... 

A slurry prepared from 100 g (0.67 mol) of p-tert-butylphenol, 35 g (ca. 1.1 mol) of paraformaldehyde (Note 1), and 2.0 mL (0.02 mol) of 10 N sodium hydroxide (Note 2) 1n 600 mL of xylene Is placed in a 2-L, round-bottomed, three-necked flask fitted with a Dean-Stark water collector and a mechanical stirrer. The air in the flask is replaced with nitrogen, and the stirred contents of the flask are heated to reflux by means of a heating mantle. After 30 min a homogeneous solution is obtained, and after 1 hr a white precipitate begins to form. The reaction mixture is refluxed for 4 hr, the heating mantle is removed, the mixture is allowed to cool to room temperature, and the precipitate is removed by filtration. The crude product Is washed, in succession, with 400-mL portions of toluene, ether, acetone, and water and is... 

Apparatus 3-1 round-bottomed, three-necked flask, equipped with a gas inlet tube, a mechanical stirrer and a powder funnel (fig. 15), the powder funnel is replaced by a vent as soon as the introduction of the metal is completed. 

Apparatus A 500-ml round-bottomed, three-necked flask, equipped with a gas inlet, a dropping funnel and a reflux condenser. The top of the condenser is connected to a washing bottle containing hexane. The inlet lube should not dip more than 0.5 cm in the hexane. The solution is stirred magnetically. All connections should be made gas-tight. 

Apparatus 300-ml round-bottomed, three-necked flask, equipped with a mechanical stirrer, a thermomether and a vent... 

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