Condensers reflux

For extraction purposes, a Soxhlet apparatus (Fig. 23(H)) can be inserted between a flask of boiling solvent and the reflux condenser A above. This apparatus is similar in design to that shown in Fig. 19, p. 3b in the type shown in Fig. 23(H) the hot extract continuously overflows through the side- tube into the boiling solvent below, but the syphon type shown in Fig. 19 is also available. 

Use the apparatus shown in Fig. 38, p. 63, using a thermometer reading to 100° and with water running through the vertical condenser. Place in the 25 ml. pear-shaped flask 5 ml. of ethanol, 5 ml. of glacial acetic acid and add carefully with shying i ml. of concentrated sulphuric acid. Attach the flask to the reflux condenser and boil the mixture gently for 10 minutes. 

Add in turn benzyl chloride (8 3 g., 8 o ml.) and powdered thiourea (5 gm.) to 10 ml. of 95% ethanol in a 100 ml. flask fitted with a reflux condenser. Warm the mixture on the water-bath with gentle shaking until the reaction occurs and the effervescence subsides then boil the mixture under reflux for 30 minutes. Cool the clear solution in ice-water, filter off the crystalline deposit of the benzylthiouronium chloride at the pump, wash it with ice-cold ethyl acetate, and dry in a desiccator. Yield, 11-12 g., m.p. 170-174°. The white product is sufficiently pure for use as a reagent. It is very soluble in cold water and ethanol, but can be recrystallised by adding ethanol dropwise to a boiling suspension in ethyl acetate or acetone until a clear solution is just obtained, and then rapidly cooling. 

Assemble in a fume-cupboard a 3-necked flask fitted with a stirrer, a reflux condenser, and a dropping-funnel, the apparatus... 

Assemble a 250 ml. three-necked flask, fitted with a stirrer, a reflux condenser and a dropping-funnel, as in Fig. 22(A) and (j), p. 43, or Fig. 23(c), p. 46 (or a two-necked flask, with the funnel fitted by a grooved cork (p. 255) to the top of the condenser). Place 40 ml. of ethanol in the flask, and then add 2-3 g. of sodium cut into small pieces. When all the sodium has dissolved, heat the stirred solution on the water-bath, and run in from the funnel 17 g. (17 ml.) of ethyl malonate and then (more slowly) io-2 g. (12 ml.) of mesityl oxide, the reaction-mixture meanwhile forming a thick slurry. Boil the stirred mixture under reflux for i hour, and then add a solution of 10 g. of sodium hydroxide in 50 ml. of water, and continue boiling the pale honey-coloured solution for ij hours more. 

Fit a three necked 250 ml. flask with a central rubber-sleeved or mercury-sealed stirrer, c/. Fig. 23(c), p. 45, where only two necks are shown, and with a thermometer the bulb of which reaches as near the bottom of the flask as the stirrer allows the third neck will carry at first a dropping-funnel and later a reflux condenser. Place 20 g. (19-5 ml.) of ethyl acetoacetate and 45 ml. of glacial acetic acid in the flask and by ice-water cooling adjust the temperature of the stirred mixture to 5 -7° maintain this temperature whilst adding a solution of 5 4 g. of sodium nitrite in 8 ml. of water slowly from the dropping-funnel during 15 minutes. Continue the stirring for 20-30 minutes, and then... 

After 3 hours, replace the separating-funnel by a reflux condenser, and the thermometer by a stopper. Add 11 g. of zinc dust in small portions by rapid removal of the stopper at such a rate that the liquid is first brought to the boil (usually about 2 portions of 2 g. each) and is then maintained gently boiling. A ooid too rapid addition of the zinc, otherwise the reaction will become too vigorous, and rapid immersion of the flask in ice-water will be necessary to control the effervescence. 

Fit a 250 ml. three-necked flask with a stirrer, a reflux condenser and a dropping-funnel. (Alternatively, use a two-necked flask, with the dropping-funnel fitted by a grooved cork into the condenser.) Place 15 g. of powdered thiourea and 40 ml. of water in the flask and stir the mixture whilst 18 5 g. (16 ml.) of chloroacetone are added dropwise over a period of 20 minutes the thiourea will dissolve and the temperature of the mixture... 

Dissolve 13 g. of sodium in 30 ml. of absolute ethanol in a 250 ml. flask carrying a reflux condenser, then add 10 g. (9 5 ml.) of redistilled ethyl malonate, and place the flask on a boiling water-bath. Without delay, add a solution of 5 3 g. of thiourea in a minimum of boiling absolute ethanol (about 100 ml.). The sodium salt of thiobarbituric acid rapidly begins to separate. Fit the water-condenser with a calcium chloride guard-tube (Fig. 61, p. 105), and boil the mixture on the water-bath for 1 hour. Cool the mixture, filter off the sodium salt at the pump and wash it with a small quantity of cold acetone. Dissolve the salt in warm water and liberate the acid by the addition of 30 ml. of concentrated hydrochloric acid diluted with 30 ml. of water. Cool the mixture, filter off the thiobarbituric acid, and recrystallise it from hot water. Colourless crystals, m.p. 245 with decomposition (immersed at 230°). Yield, 3 5 -4 0 g. 

Acetylation. Place 1 ml. of the substance (or, if solid, i g. of the powdered amine) in a small flask fitted with a reflux condenser (or in a test-tube fitted with a cold-finger, as in Fig. 35, p. 62), add 5 ml. of an acetic anhydride-acetic acid mixture (equal volumes) and reflux... 

The use of reflux condensers during the acetylation is not absolutely essential, since very little evaporation of the acetylating mixture from an open conical flask would occur during heating on the water-bath. The use of... 

Multi-necked flasks. Fig. II, 1, 8, a, illustrates a typical threenecked flask. This has numerous applications in organic chemistry for many operations, the central aperture carries a mechanical stirrer, and the two side apertures a dropping funnel and a reflux condenser respectively. 

A modified Hempel column, which incorporates a small reflux condenser ( cold finger or cold spot condenser ), is shown in Fig. 11,... 

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. 

If preferred, the following alternative procedure may be adopted. The absolute alcohol is placed in a 1 5 or 2 litre three-necked flask equipped with a double surface reflux condenser and a mercury-sealed mechanical stirrqr the third neck is closed with a dry stopper. The sodium is introduced and, when it has reacted completely, the ester is added and the mixture is gently refluxed for 2 hours. The reflux condenser is then rapidly disconnected and arranged for downward distillation with the aid of a short still head or knee tube. The other experimental details are as above except that the mixture is stirred during the distillation bumping is thus reduced to a minimum. 

Ammonia. Small quantities of ammonia may be prepared with the aid of the apparatus depicted in Fig. II, 48,4. Concentrated ammonia solution (sp. gr. 0-88) is gently heated in the flask surmounted by an efficient reflux condenser. The gas is dried by passage through the tower which is loosely packed with soda lime or quicklime, and is then passed... 

Beginnera may prefer to fit the flask with a reflux condenser and thus considerably reduce the danger of fire. 

The swan neck adapter of Fig. II, 56, 12 is useful for distillations as it permits the use of a capillary tube (held in position by a short length of heavy-walled rubber tubing) not sealed to a ground joint. It may also be used for inser tion of a thermometer or a gas-inlet tube in the narrow neck and a reflux condenser into the ground joint this device virtually converts a three-necked into a four-necked flask. Common sizes are cone fil9, 24, 29, or 34 socket 19, 24 or 29. 

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