Adapter, Claisen vacuum

Fig. I-I (com.) (z) Claisen distilling head with Vigreux column (aa) Graham condenser (bb) West condenser (cc) Allihn condenser (dd) Friedrichs condenser (ee) collecting adapter (ff) vacuum adapter (gg) straight vacuum adapter.

Setup your glassware for simple distillation with a claisen adapter, three way adapter, pressure-equalized addition funnel, water cooled condenser, vacuum adapter and receiver flask to catch any condensed solvent vapors. 

Claisen distilling links with standard ground joints, Liebig condenser with vertical delivery tube and vacuum adapter and pig receiver for three flasks... 

Prelab Exercise Study the glassware diagrams and be prepared to identify the fractionating column, Claisen distilling hjead, ordinary distilling head, vacuum adapter, simple bent adapter, calcium chloride tube, Hirsch funnel, and Buchner funnel. 

A typical vacuum distillation apparatus is illustrated in Fig. 1. It is constructed of a round-bottomed flask (often called the pot ) containing the material to be distilled, a Claisen distilling head fitted with a hair-fine capillary mounted through a rubber tubing sleeve, and a thermometer with the bulb extending below the side arm opening. The condenser fits into a vacuum adapter that is connected to the receiver and, via heavy-walled rubber tubing, to a mercury manometer and thence to the trap and water aspirator. 

Fig, 102 k Claisen adapter so you con vacuum distill and take temperatures too. 

Connecting to Vacuum. In Figure 16.1, the connection to vacuum has been made using a multipurpose adapter (see Technique 14, Figure 14.9B). If a multipurpose adapter is not available, an alternative method uses a Claisen head and two thermometer adapters (Figure. 16.2). If two thermometer adapters are not available, a 0 rubber stopper fitted with glass tubing can be used. 

A vacuum distillation apparatus using the components of the traditional organic laboratory kit is shown in Figure 16.5. It uses the ebulliator tube, the Claisen head, and a thermometer for internal temperature monitoring. A water condenser is shown, but with high-boiling liquids, this apparatus may be simplified by removing the water condenser. A special vacuum adapter allows connection to the manometer and vacuum source. 

Apparatus A 25-mL round-bottom flask, Claisen adapter, rubber septum, drying tube, two 1-mL syringes and a 5-mL syringe with needles, cold-water bath, apparatus for magnetic stirring, vacuum filtration, and flameless heating. 

Work-Up and Isolation Remove the Claisen adapter from the vial, and add 1 mL of water with stirring. Collect the precipitated product by vacuum filtration, wash it with cold 1 1 methanol-water, and air-dry it. Recrystallize the crude stilbene from 95% ethanol. 

Work-Up and Isolation Remove the gas trap, separatory funnel, condenser, and Claisen adapter from the reaction flask. Add 15 mL of 2.5 M aqueous sodium hydroxide to the stirred solution and continue stirring for 15 min swirl the flask if necessary to dissolve all of the white solid. Transfer the reaction mixture to a separatory funnel, separate the layers, and remove the lower aqueous layer. Wash the organic layer with 15 mL of cold3 M hydrochloric acid, venting as necessary, and then with 15 mL of cold water. Dry the organic layer over several spatula-tips full of anhydrous sodium sulfate." Filter or carefully decant the solution into a tared round-bottom flask and remove most of the ether by simple distillation. Alternatively, use rotary evaporation or other techniques to concentrate the solution. The final fraces of solvent may be removed by conneoting the cool stillpot to a vacuum source. Determine the yield of crude producf." ... 

Into a lOOmL one-necked round-bottomed flask is placed 20 mesh tin powder (1.5 g). The flask is clamped to a ring stand or other support, and placed on a 100 mL heating mantle. The flask is fitted with a reflux condenser topped with a Claisen adapter, and the reflux condenser is attached with rubber or plastic tubing to a cold water tap and a drain. The straight neck of the Claisen adapter is stoppered, and the curved neck is fitted with a gas inlet adapter (either a vacuum... 

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