Pumps water aspirator

A source of vacuum, usually a water pump (water aspirator) which is connected to the receiving flask by thick walled rubber tubing (pressure tubing). Sometimes there will be a trap between the water pump and the receiving flask. 

Material Round flask with outlet, stopper and stop cock, syringe, water jet-pump (water aspirator), large glass bowl. 

A solution of 30 g (0.1 mole) of 17j5-hydroxy-5a-androstan-3-one (androstano-lone), 20 ml of pyrrolidine and 200 ml of benzene is heated at reflux temperature for 2.5 hr under a Bidwell-Sterling water trap. The benzene solution is evaporated to dryness in a rotating evaporator connected to a water aspirator. The white cake which remains is broken up and dried further by immersing the flask in a water bath at 60-75° and evacuating the flask with a mechanical vacuum pump. After 0.5 hr the solid cake is broken up again and dried for another 0.5 hr at 60-75°. The enamine (9) obtained should smell only faintly of pyrrolidine. 

Beakers 10 to 1000-ml. volumetric flasks 1-ml. volumetric pipet, serological pipet steam bath vacuum desiccator vacuum pump and water aspirator are also required. 

Considerable dissolved hydrogen chloride is liberated at this point and passes into the water aspirator. A mechanical vacuum pump should not be used at this stage because it would be damaged by corrosion. 

B. Pyridine-N-oxide. The acetic acid solution is evaporated on the steam bath under the pressure of a water aspirator, and the residue (180-190 g.) is distilled at a pressure of 1 mm. or less in an apparatus suitable for collecting a solid distillate (Note 5). The vacuum pump must be protected with a Dry Ice trap capable of holding about 60 ml. of acetic acid, which distils as the pyridine-N-oxide acetate dissociates at low pressure. Heat is provided by an oil bath, the temperature of which is not allowed to rise above 130° (Note 6). The product is collected at 100-105°/1 mm. (95-98°/0.5 mm.). The yield is 103-110 g. (78-83%) of colorless solid, m.p. 65-66° (sealed capillary). The base is deliquescent and must be stoppered immediately. 

A 1-1., three-necked, round-bottomed flask equipped with a Trubore stirrer, a pressure-equalizing dropping funnel, and a reflux condenser with a drying tube is charged with 350 ml. of acetonitrile (Note 1) and 106.4 g. (0.41 mole) of triphenylphos-phine (Note 2). The flask is cooled in an ice-water bath (Note 3), and 64 g. (0.40 mole) of bromine is added dropwise over a period of ca. 15-20 minutes (Notes 4 and 5). The ice-water bath is removed, and a solution of 54 g. (0.40 mole) of cinnamyl alcohol in 50 mi. of acetonitrile is added in portions over a period of 5-10 minutes with continued stirring (Note 6). The solvent is removed by distillation with the use of a water aspirator (30-40 mm.) and an oil bath until the bath temperature reaches 120°. The water aspirator is replaced by a vacuum pump and the water-cooled condenser with an air condenser, and the distillation is continued with rapid stirring (Notes 7, 8, and 9). Most of the product (Note 10) distills at 91-98° (2-4 mm.), and about 59 g. of product crystallizes in the receiving flask (63-75% yield) (Note 11). 

The vacuum adapter is connected to a vacuum source, either a vacuum pump or a water aspirator. Real live vacuum pumps are expensive and rare and not usually found in the undergraduate organic laboratory. If you can get to use one, that s excellent. See your instructor for the details. The water aspirator is used lots, so read up on it. 

After this period, the dropping funnel and the vacuum takeoff are replaced by the short-path distillation assembly shown in Figure 2. The system is protected by a Drierite tube and the benzene is distilled under reduced pressure (water aspirator). After the benzene is removed, the benzene-containing receiver is replaced with a clean, dry flask, and the system is connected to an eflScient vacuum pump. The pressure in the system is reduced to 0.02 mm., and the flask is immersed deeply in an oil bath (Figure 2) heated to about 200°. After about 1 ml. of fluid forerun is collected, the diethylaluminum cyanide distils at 162° (0.02 mm.) (Note 7) and is collected in a tared 200-ml. receiver by heating the side arm and the adaptor with a stream of hot air or an infrared lamp (Note 8). After all the distillate is collected in the receiver (Note 9), dry nitrogen is admitted to the evacuated apparatus and the receiver is stoppered and weighed. Diethylaluminum cyanide is obtained usually as a pale yellow syrup (Note 10) in 60-80% yield (26.7-35.6 g.) (Note 11). 

Rotary evaporator with vacuum pump or water aspirator, 40°C... 

Rotary evaporator with water aspirator or vacuum pump, 40°C water bath... 

Place the filtered proanthocyanidin extract into an appropriately sized round-bottom flask and remove acetone on a rotary evaporator equipped with a water aspirator or vacuum pump, at 40°C. 

Better yields are obtained at low pressures (preferably below 5 mm.) because of more efficient sublimation of coumalic acid. The submitters report that a water aspirator could be used with crude (unrecrystallized) coumalic acid to avoid damage to the vacuum pump by untrapped corrosive vapors, and that yields of a-pyrone averaged 45% in this modification. The checkers used a mechanical pump with an efficient sodium hydroxide trap in all runs. 

A.M. Russel, Use of Water Aspirator in Conjunction with Sorption Pumping on an... 

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