98 
Journal of the Mitchell Society 
[November 
bath of cottonseed oil . At 220° copious evolution of ammonia be- 
gan . The gas, dried over quicklime, was passed through the benzene 
solution of the ethoxy compound for forty-five minutes, during 
which time the temperature of the oil bath was gradually raised to 
245°. 
The benzene solution was placed in a 50 cc. round bottom flask 
provided with a three-hole rubber stopper through which passed 
a thermometer dipping into the solution and the inlet and outlet 
tubes for the ammonia. 
Experiment A: The initial temperature of the benzene solution 
was 22°. When the temperature of the oil bath surrounding the 
generator reached 220° the temperature in the absorption flask 
began to rise. After five minutes it was 25°, after ten minutes 
33°, after fifteen minutes, 38°. Meanwhile the yellow color of the 
original solution gradually faded. After twenty minutes the tem- 
petature was 40°, then suddenly the separation of the white sub- 
stance took place to such an extent that the mass became almost 
solid . A portion of the substance was at once removed from the 
absorption flask, pressed between folds of drying paper and dis- 
solved in water. No evidence of hydrolysis could be detected, the 
solution being perfectly neutral to indicators, As Rosenheim 
found that his salt was strongly hydrolyzed, it was decided to con- 
tinue the passage of the ammonia gas into the crystal broth longer. 
Accordingly, this was continued for twenty-five minutes more, the 
temperature of the solution falling gradually. The vessel tightly 
corked was allowed to stand two weeks. At the end of this time 
the crystals were filtered from the benzene and pressed between 
folds of drying paper, then recrystallized from absolute alcohol 
and labeled “A”. 
Experiment B : This was a repetition of Experiment A except 
that the crystals were removed from the benzene immediately after 
the conclusion of the experiment. The maximum temperature 
observed in the absorption flask was 44° . The separation of the 
crystals took place twenty-two minutes after the temperature of 
the oil bath surrounding the ammonia generator had reached 220°. 
The substance recrystallized from alcohol was labeled “B”. 
