Organic Syntheses, CV 6, 731
2. It is necessary to use a dry ice condenser to shorten the time required to condense the ammonia (4 hours compared with 6 hours without the condenser). The ammonia tank was warmed with an air gun during the distillation. The condenser was removed after the ammonia was collected.
3. It is necessary to use a strong stirring motor since the reaction mixture becomes, temporarily, rather viscous.
4. One should not pour the liquified ammonia directly out of the cylinder since particles of iron compounds might be carried along, catalyzing the formation of sodium amide. For the exclusion of moisture it is also necessary to use a drying tower (potassium hydroxide) between the cylinder and the flask.
5. The sodium should be cut into small particles to increase the speed of dissolution and diminish the danger of stirrer blockage.
6. During this period the reaction mixture might turn white. In this case, another portion of sodium must be added until the solution becomes blue again.
Organic Syntheses, CV 5, 467
3. Only five or six pieces of sodium should be added at one time in order to avoid an almost uncontrollable exothermic reaction. The solution turns blue and then white as the sodium is consumed. When the solution turns white, another portion of sodium may be added. The last 50 g. of sodium may be added without waiting between portions because the reaction is much slower at this point.
4. Because dissolution of the salts is a highly exothermic process, the water should be added slowly. A stream of nitrogen may be passed through the reaction during the addition of the water to ensure that no fire is started by bits of sodium that may be adhering to the upper walls of the flask.
Organic Syntheses, CV 4, 887
5. During the addition of the lithium the solution turns deep blue. After this has occurred (after about one-third of the lithium has been added), the rate of addition can be increased considerably.