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Laboratory Methods of Organic Chemistry - Sciencemadness Dot Org

Laboratory Methods of Organic Chemistry - Sciencemadness Dot Org

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CHAPTBE I<br />

THE REPLACEMENT OF HYDROXYL AND HYDROGEN<br />

BY HALOGEN<br />

ALCOHOLS AND OLEFINES<br />

1. ETHYL BROMIDE FROM ETHYL ALCOHOL<br />

ALCOHOL (110 c.c. ; 90 g. <strong>of</strong> 95 per cent) is rapidly poured with<br />

continuous shaking but without cooling into a round-bottomed flask<br />

(capacity about 1 1.) containing 200 g. (110 c.c.) <strong>of</strong> concentrated<br />

sulphuric acid ; the warm mixture is then cooled to room temperature,<br />

75 g. <strong>of</strong> ice-water are cautiously added with continued cooling,<br />

FIG. 46<br />

and finally 100 g. <strong>of</strong> finely powdered potassium bromide are dropped<br />

in. The reaction mixture is then heated on a small sand bath over<br />

a powerful flame so that a fairly rapid distillation takes place.<br />

Since the ethyl bromide has a low boiling point the longest condenser<br />

available is used along with an adapter or else a coil condenser<br />

(Kg. 46), and a really rapid current <strong>of</strong> water is passed through.<br />

Before the distillation is begun sufficient water is poured into the<br />

receiver to submerge the end <strong>of</strong> the adapter and a few pieces <strong>of</strong> ice<br />

93

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