Distillation columns Widmer

NOTE The original procedure [35] calls for the use of a Widmer column for the fractional distillation step. Since this piece of equipment is no longer generally available and discredited by some experts in laboratory fractional distillations, we suggest the use of a single-turn, glass-helix packed distillation column or its equivalent with a total-reflux, partial-take-off distillation head. 

Fractional distillation. Fig. II, 60, 2 illustrates a set-up for fractional distillation wdth a Hempel-type column and cold finger, the latter to give manual control of the reflux ratio. Any other fractionating colunm, e.g., an all-glass Dufton or a Widmer column may, of course, be used. 

Pour the reaction mixture cautiously into 400 g. of crushed ice and acidify it in the cold by the addition of a solution prepared by adding 55 ml. of concentrated sulphuric acid to 150 ml. of water and then coohng to 0°. Separate the ether layer and extract the aqueous layer twice with 50 ml. portions of ether. Dry the combined ethereal solutions over 50 g. of anhydrous potassium carbonate and distil the filtered solution thror h a Widmer column (Figs. II, 17, 1 and II, 24, 4). Collect separately the fraction boihng up to 103°, and the dimethylethynyl carbinol at 103-107° Discard the high boiling point material. Dry the fraction of low boihng point with anhydrous potassium carbonate and redistil. The total 3 ield is 75 g. 

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. 

Widmer column. The remaining liquid was also distilled at normal pressure, using... 

A solution of (CH3)3C-CH=C=CLi, obtained by addition at -60°C of 0.20 mol of tert.-butylallene (see Chapter VI, Exp. 2) to a solution of 0.25 mol of ethyllithium in about 200 ml of diethyl ether (see Chapter II, Exp. 1) was warmed to 25°C and held at this temperature for 15 min. Subsequently the solution was cooled to below 0°C and 50 ml of saturated NH,C1 solution were added dropwise with vigorous stirring, keeping the temperature below 2o C. The upper layer v as separated off and the aqueous layer was extracted twice with 25-ml portions of diethyl ether. The combined solutions were dried over a small amount of magnesium sulfate. Slow distillation through a 40-cm Widmer column gave neopentyl acetylene (b.p. 76°C/750 mmHg, 20... 

Widmer column gave butylallene, b.p. 105 C/760 mmHg, n 1.4332. The remaining liquid was distilled in a partial vacuum (60-100 mmHg, b.p. 40-70°C) and the distillate was redistilled at normal pressure to give an additional amount of butylallene, bringing the yield to 72-78%. 

After cooling to about 40°C (note 2) the viscous brown liquid was poured into a vigorously stirred solution of 50 g of ammonium chloride in 250 ml of 4 N HCl, which was kept at 0-5°C. The flask was also rinsed with this solution. The product was extracted 5-7 times with a 1 1 mixture of diethyl ether and pentane. The combined extracts were washed with saturated NHi Cl solution and subsequently dried over magnesium sulfate. The residue remaining after removal of the solvents in a water-pump vacuum, was carefully distilled through a 30-cm Widmer column. The desired nitrile, b.p. 84°C/15 mmHg, n 1.4487, was obtained in 72% yield. The first fraction (about 5 g) consisted mainly of the 1,3-substitution product n-C,HgC(CsN)=C=CH2. 

N32C03, water, dried (Na2S04) and distilled several times in a vac through a Widmer Helv Chim Acta 7 59 1924) or Vigreux column [Wicterle and Hudlicky Collect Czech Chem Commun 12 564 1947 Hagemeyer and Hull Ind Eng Chem 41 2920 1949]. 

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