Tubes drying

Liberation of iodine on heating. On heating in a dry tube, iodoform gives off copious violet vapours of iodine. This will have been observed during the Preliminary Tests, p. 319. 

Weigh the clean dry tube T, then add about 25 ml. of the pure solvent (i.e., sufficient to ensure that the bulb of the thermometer... 

Two forms of the so called calcium chloride tubes (also termed drying tubes, straight form) are shown in (c) and (d) these are fiUed with anhydrous calcium chloride or with cotton wool (previously dried at 100°), and are attached by means of a stopper to a flask or apparatus containing substances from which moisture is to be excluded. 

Fig. 77,13, 1 illustrates a distillation unit when it is desired to protect the distillate from moisture in the atmosphere. The drying tube may be filled with anhydrous calcium chloride held in position by loose plugs of glass wool or with a loose plug of cotton wool. Fig. 77,13, 2 depicts the use of an air condenser for liquids of boiling point above 140-150°. 

Absorbent cotton (cotton wool). This material is an excellent drying agent for use in the so-called calcium chloride tubes, i.e., drying tubes, placed at the top of dropping funnels, reflux condensers, etc., to exclude moisture. It is more convenient than calcium chloride, and should preferably be dried in an oven at 100° before use. 

Receiver adapters or connectors. Various forms of receiver adapters are shown in Figs. 11, 56, 26-29. The simplest form. Fig. 11, 56, 26, carries a glass hook for securing it to the condenser by means of a rubber band from the side tube to the hook an improved form, incorporating two ground glass joints is shown in Fig. 11, 56, 27. A useful adapter is illustrated in Fig. 11, 56, 28 when employed at atmospheric pressure, a drying tube may be attached to the side tube, if desired in a distillation under reduced pressure, the side tube is connected to the pump. Fig. 11, 56, 29 depicts a receiver adapter with an additional socket connection. 

Method B. In a 500 ml. round-bottomed flask, provided with a reflux condenser protected by a cotton wool (or calcium chloride) drying tube, place 59 g. of succinic acid and 102 g. (94-5 ml.) of redistilled acetic anhydride. Reflux the mixture gently on a water bath with occasional shaking until a clear solution is obtamed ca. 1 hour), and then for a further hour to ensure the completeness of the reaction. Remove the complete assembly from the water bath, allow it to cool (observe the formation of crystals), and finally cool in ice. Collect the succinic anhydride as in Method A. The yield is 45 g., m.p. 119-120°. 

Mix together in a 250 ml. flask carrying a reflux condenser and a calcium chloride drying tube 25 g. (32 ml.) of freshly-distilled acetaldehyde with a solution of 59-5 g. of dry, powdered malonic acid (Section 111,157) in 67 g. (68-5 ml.) of dry pyridine to which 0-5 ml. of piperidine has been added. Leave in an ice chest or refrigerator for 24 hours. Warm the mixture on a steam bath until the evolution of carbon dioxide ceases. Cool in ice, add 60 ml. of 1 1 sulphuric acid (by volume) and leave in the ice bath for 3-4 hours. Collect the crude crotonic acid (ca. 27 g.) which has separated by suction filtration. Extract the mother liquor with three 25 ml. portions of ether, dry the ethereal extract, and evaporate the ether the residual crude acid weighs 6 g. Recrystallise from light petroleum, b.p. 60-80° the yield of erude crotonic acid, m.p. 72°, is 20 g. 

Coumarin. In a 250 ml. round-bottomed flask, provided with a small reflux condenser and a calcium chloride drying tube at the top, place 2 1 g, of salicylaldehyde, 2 0 ml. of anhydrous triethylamine and 5 0 ml. of acetic anhydride, and reflux the mixture gently for 12 hours. Steam distil the mixture from the reaction flask and discard the distillate. Render the residue in the flask basic to litmus with solid sodium bicarbonate, cool, filter the precipitated crude coumarin at the pump and wash it with a little cold water. Acidify the filtrate to Congo red with... 

To prepare crystalline monoperphthalic acid, place the thoroughly dry ethereal solution (4) in a distilling flask equipped with a capillary tube connected with a calcium chloride or cotton wool drying tube, and attach the flask to a water pump. Evaporate the ether without the application of heat (ice will form on the flask) to a thin syrup (about 150 ml.). Transfer the syrup to an evaporating dish, rinse the flask with a little anhydrous ether, and add the rinsings to the syrup. Evaporate the remainder of the ether in a vacuum desiccator over concentrated sulphuric acid about 30 g. of monoperphthalic acid, m.p. 110° (decomp.), is obtained. 

Place 65 g. of clean dry zinc wool and a few crystals of iodine in a 2 5 htre three-necked flask, equipped with an efficient reflux condenser with drying tube, a mechanical stirrer, and a dropping funnel. Prepare a mixture... 

Alternatively, use the following procedure in which triethylamine replaces potassium acetate as the basic catalyst. Place 2 1 g. (2-0 ml.) of purified benzaldehyde, 2 0 ml. of anhydrous triethylamine and 5 0 ml. of A.R. acetic anhydride in a 200 ml. round-bottomed flask, equipped with a short reflux condenser and a calcium chloride drying tube. Boil the solution gently for 24 hours—heating may be interrupted. Incorporate a steam distillation apparatus in the flask and steam distil until the distillate is no longer cloudy (about 100 ml.) and then collect a further 50 ml. of the distillate di ard the steam distillate. Transfer the residue in the flask to a 400 ml. beaker, add water until the vplume is about 200 ml., then 0 2 g. of decolourising carbon, and boil for a few minutes. Filter the hot solution, and acidify the hot filtrate with 1 1 hydrochlorioiaoid... 

Stage one - the reaction happens in the form of a reflux with a dry set-up. You will need a 2000ml reaction flask, a condenser and a drying tube packed with calcium chloride or other drying agent. The reaction needs to be stirred in a big way, so before we add the ingredients make sure you have a clean stirrer bar ready, I prefer the eggy shape bars as they tend to be less noisy. 

There s no real order needed to get the stuff into the reaction flask. Use a 1000ml flask with a stirrer bar and it s easier if the chloroform goes in last so you can wash down the solids if you have any stuck in the funnel. Set up the condenser and drying tube as we did with the methylenation. 

Apparatus 3-1 round-bottomed, three-necked flask, provided with a dropping funnel, a mechanical stirrer and a reflux condenser, cooled with dry-ice and acetone (cold finger). The upper end of this condenser was connected with a drying tube filled with anhydrous calcium chloride. 

C/760 mmHg) sulfur dichloride After the addition stirring v/as stopped and the flask was allowed to stand for 15 h in the ice-bath. The condenser was replaced with a drying tube containing CaCl (refluxing of the vinyl chloride had stopped completely after the addition of sulfur dichloride). 

Apparatus 500-ral three-necked, round-bottomed flask, provided with a dropping funnel, a gas-tight mechanical stirrer and an efficient reflux condenser a trap and a tube filled with anhydrous calcium chloride were placed between the condenser and the water pump in such a way that during the reaction the vapour of the product entered the large annular space of the trap (see Exp. 24) the drying tube was placed between the trap and the water pump. 

Apparatus-. 500-ml round-bottomed flask with a combination of thermometer and vent, connected to a drying tube filled with lumps of anhydrous calcium chloride. 

The proper volume of acetylene is measured with a water gasometer as described in Ovg. Synth., Colleat. Vol. 1 1941, 230, with two modifications (a) Two traps immersed in an acetone-dry ice bath at -65°C are placed between the acetylene tank and the gasometer in order to remove acetone. (b) The washing bottles between the gasometer and the reaction flask are replaced by a drying tube (2 x 30-cm column packed with anhydrous CaCl2). 

B. Ethyl l-( p-methoxyphenyl I-2-oxoayotohexaneaar hoxylate. A 250 mL, one-necked, round-bottomed flask, equipped with a magnetic stirring bar, is charged with 22.2 g (45 mmol) of p-methoxyphenyl 1 ead triacetate, 10.8 g (135 mmol) of pyridine (Note 8), and 70 mL of chloroform (Note 9). To this solution 1s added 7.0 g (41 mmol) of ethyl 2-oxocyclohexanecarboxylate (Note 10), a calcium chloride drying tube Is put 1n place, and the mixture is stirred at 40°C (Note 11). 

A. l-THmethyleilyloxyayalopentsne. A 1-L, two-necked, round-bottomed flask is equipped with a mechanical stirrer and a reflux condenser having a drying tube (calcium chloride). The flask is charged with 200 mL of dimethylformamide (Note 1), 45 g (0.54 mol) of cyclopentanone (Note 2), 65.5 g (0.6 mol) of chlorotrimethylsilane (Note 2) and 185 mL (1.33 mol) of triethylamine (Note 1), and the mixture is refluxed for 17 hr (Note 3). The mixture is cooled, diluted with 350 mL of pentane, and washed four times with 200-mL portions of cold saturated aqueous sodium hydrogen carbonate. The... 

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