Organic 2 Review Problem 243

Organic 2 Review Problem 243 - PREPARATIONS 227 add slowly...

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PREPARATIONS 227 add slowly 70 ml. of formic acid down the condenser, and then boil the mixture under reflux for i\ hours, during which time carbon dioxide is steadily evolved. Cool the solution thoroughly in ice-water, and then make it alkaline by the cautious addition (with stirring or shaking) of a solution of 80 g. of sodium hydroxide in ca . 150 ml. of water. Now isolate the free tertiary amine by steam-distillation into hydrochloric acid, etc., precisely as for the primary amine in Stage (D), but preferably using a smaller flask for the final dis- tillation. Collect the 2-dimethylamino-n-octane, b.p. 76-78°/15 mm. Yield, 13-14 g. At atmospheric pressure the amine has b.p. 187-188°. The hydrochloride of the amine may be prepared precisely as that of the primary amine. For recrystallisation, boil a suspension of the powdered salt in petroleum (b.p. 60-80°), and then add acetone slowly in small drops until the boiling suspension just becomes clear: allow the stirred solution to cool until
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This note was uploaded on 09/19/2011 for the course CHM 2211 taught by Professor Castalleano during the Fall '06 term at University of Florida.

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