Vigreux

Fig. II, 16, 1 illustrates a set-up for simple fractionation a Hempel column is shown, but it may be substituted by a modified Hempel, a Vigreux or an all-glass Dufiton column. The Hempel column may be filled with glass rings, h porcelain Lessing rings, or with porcelain rings. The mixture to be fractionated is placed in a bolt - head flask of convenient size (it should be one third to one half full), a few fragments of porous porcelain added, the column fixed in position, and a water condenserattacfied to the side arm. The distillate is collected in small flasks or in test tubes. The bulb of the thermometer should be just below the level of the side arm.

Any fractionating column of moderate efficiency is satisfactory, e.g., a Dufton column (20 cm. long containing a spiral 10 cm. in length, 2 cm. in diameter with 8 turns of the helix) or a Vigreux column (20-25 cm. long). 

Alternatively, an independent column (Fig. XII, 2, 8, c) may be inserted into a flask the column may be of the Vigreux, Widmer or Hempel form. The fractionating column should be lagged with asbestos cloth or string for distillation temperatures above 100° for the best results the column should be heated electrically (compare Section 11,15) to a temperature 5-10° below the b.p. of the fraction being collected. The side arm of the flask or fractionating column may be attached to a cold spot condenser and receiver as in Fig. XII, 2, 4 or to a Liebig s condenser and receiver as in Fig. XII, 2, 1. 

Appamtus 2-1 two-necked, round-bottomed flask, provided with a stopper and a 40-cm Vigreux column. This column was connected to a descending condenser and a receiver, fl tube filled with KOH pellets was placed betv/een the water pump and the receiver. 

The aqueous layer was extracted with diethyl ether. The combined ethereal solutions were dried over potassium carbonate, after which the greater part of the diethyl ether was distilled off at normal pressure through a 40-cm Vigreux column (bath temperature < 90°C). Careful distillation of the remaining liquid afforded the bis-ether, b.p. 47-49°C/18 mmHg, Op 1.4469, in 78% yield. 

The residue was distilled through a 30-cm Vigreux column, giving the desired... 

The combined solutions were dried over magnesium sulfate and subsequently concentrated in a water-pump vacuum. Distillation of the residue through a 30-cm Vigreux column gave the silylated propargyl sulfide, b.p. 65°C/18 mmHg, n ... 

HCl and 50 ml of water. The upper layer was separated off and the aqueous phase was extracted five times with small portions of THF. After drying the combined solutions over magnesium sulfate the solvent was removed in a water-pump vacuum. The residue was distilled through a 30-cm Vigreux column, connected to an air condenser. After a preliminary aqueous fraction of the carboxylic acid the main fraction passed over at 100°C/15 mmHg. The compound solidified in the receiver and (partly) in the condenser. The yield was almost quantitative. 

Vigreux column gave the enyne alcohol, b.p. 75 C/15 mmHg, n 1.4955, in 55-7451 yield. 

To a vigorously stirred suspension of 2 mol of lithium amide in 2 1 of liquid atimonia (see II, Exp. 11) was added in 15 min 1 mol of propargyl alcohol (commercial product, distilled in a partial vacuum before use). Subsequently, 1 mol of butyl bromide was added dropwise in 75 min. After an additional 1.5 h, stirring was stopped and the ammonia was allovied to evaporate. To the solid residue were added 500 ml of ice-water. After the solid mass had dissolved, six extractions with diethyl ether were performed. The (unwashed) combined extracts were dried over magnesium sulfate and then concentrated in a water-pump vacuum. Distillation of the residue through a 40-cm Vigreux column afforded 2-heptyn-l-ol, b.p. 

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