104 Journal of the Mitchell Society \_N 0 ve 7 nber 
ski and Orzechowski 1 prepare this compound without the use 
of any solvent. They use an excess of chloral and get sev- 
eral by-products. We have tried their method but have 
employed theoretical proportions. Even so we get the same 
by-products. We set the mortar in a block of ice and rapidly 
stirred together the previously cooled substances. The mix- 
ture liquefied and then rapidly became very hard. This pro- 
duct decomposed at about 127°, after two hours on ice at 124° 
and after three hours more at room temperature at 118°. It 
was rubbed up with a little water and filtered. The decom- 
position point rose to 135°. Now taking advantage of the 
marked difference in solubility in benzene of the mono- and 
di-compounds (not observed by Niementowski) we extracted 
the crystalline mass, weighing 8.2 grams, with 45cc boiling 
benzene. From the extract there separated a mass of color- 
less needles, weighing 3.7 grams and melting 149°-152°, 
hence nearly pure mono-compound. On evaporating the fil- 
trate a residue was obtained, weighing 1.3 grams and melting 
at 160°, a good quality of the di-compound. A second ex- 
traction was made with 33cc of boiling benzene. On cooling 
this yielded a product weighing 0.8 gram and melting at 162°, 
and a residue at 157°. There still remained an insoluble 
residue, dark purple in color. These results are in marked 
contrast to those obtained by our method of boiling in ben- 
zene, for we get practically only the mono-compound and 
consequently a much larger yield. 
Anplysis: 
0.2000 gram substance gave 0.3189 gram AgCl. 
Calculated for 
C 9 H 6 0 2 NC1 3 Found 
Cl 39.92 39.43 
On treating a glacial acetic acid solution of this compound 
with bromine a bromo derivative is obtained in large quan- 
tity. On cooling a hot glacial acetic acid solution it deposits 
i(Ber. 28, 2812). 
