LABORATORY SYNTHESIS OF ETHYL CHLOR.IDE I. A. KOTEN North Central College, Naperville, Illinois
THE following procedure is suggested as being rapid and convenient for the laboratory or lecture preparation of ethyl chloride: T Into a 500-ml. flask ( A ) place 150 ml. of 95 per cent alcohol and 25 g. of anhydrous calcium chloride. Shake the mixture until practically all of the calcium fiO-' chloride is dissolved, and then add 35 g. of ethyl sulfate (E. K. Practical). Place the flask on the water bath and connect with the 250-ml. flask (B), which . contains 75 ml. of concentrated HzS04. Connect with the condenser immersed in a freezing mixture of salt and ice. The liquefied ethyl chloride drops into the ary product appears as a precipitate. The ethyl chloreceiving flask ( C ) , which is also packed in a cooling ride thus obtained is always of interest to students, mixture. The temperature of the freezing mixture who note the extreme cooling effect produced upon should be about - 10°C. After the flasks have been pouring this compound over the hack of the hand. securely connected the temperature of the water bath is The yield of pure ethyl chloride based on the calgradually raised to 70°C. and kept there for the dura- cium chloride used according to the reaction: tion of the preparation, which is usually about half an CaCL (C3HJzS0, C2Hi304CaCI C2HaC1 hour. Upon warming the mixture in flask A copious evolution of ethyl chloride begins. The compound averages 63 per cent. One ethyl radical of diethyl in its 'gaseous state is bubbled through concentrated sulfate reacts more vi~orouslythan the other.' , H2S0, in order to free i t from alco% vapors and ,CAD=, A,, "Commeiial ethylation with diethyl sulfate." moisture. After the reaction is completed the second- C h m . and Met. Eng.. 29, 319 (1923).
+
-
+
