Organic 2 Review Problem 119

Organic 2 Review Problem 119 - PREPARATIONS 103 25 ml. (20...

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PREPARATIONS 103 25 ml. (20 g.) of fl-butanol in a 250 ml. round-bottomed flask, and then fit a dropping-funnel to the flask through a cork which has a groove cut or filed in the side (as F in Fig. I(B), p. 3) to allow escape of air. Place 25 ml. of concentrated sulphuric acid in the funnel, and then allow the acid to fall slowly dropwise into the flask, keeping the contents well shaken meanwhile and cooled occasionally in an ice-water bath. When the addition is complete, replace the funnel with a reflux water- condenser, and then gently boil the mixture over a sand-bath for ca. 45 minutes, shaking the flask gently from time to time. Then remove the reflux condenser, and fit a "knee-tube" and condenser to the flask as shown in Fig. 59, p. ioo or Fig. 23(0), p. 45, and distil off the crude n-buryl bromide (ca. 30 ml.). Purify the distillate by first shaking it with water in a separating-funnei: run off the lower layer of bromide, reject the aqueous layer, and then return the bromide to the funnel and shake
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