Carbon dioxide recovery, amine solution

Eleven and five-tenths grams (0.50 gram atom) of sodium is added in small portions to a stirred solution of 0.15 g. of powdered ferric nitrate in 300 ml. of liquid ammonia. (Hood.) The reaction mixture is cooled in a solid carbon dioxide-ethanol bath during this and subsequent operations. After the blue color of liquid ammonia solution is discharged (15-20 minutes after addition of the sodium), the temperature of the reaction mixture is adjusted to —50° and 53 g. (0.50 mole) of isoamyl chloride is added at the rate of 30-4 0 drops per minute. Stirring is continued for 1 hour after completion of the addition. The excess ammonia is then allowed to evaporate slowly, and the residue is hydrolyzed by the dropwise addition of excess water. Twenty grams of sodium hydroxide is then added, and the mixture is extracted with ether. Distillation of the ether followed by fractionation of the residual liquid gives a 40% yield of 3-methyl-l-aminobutane with a 10% recovery of alkyl chloride. The amine boils at 95°. 

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