84 
Bromoform. 
Am.  Jour.  Pha 
Feb.,  1891. 
laroi. 
remaining  precluded  any  further  investigation.  The  fractions 
obtained  between  100°  and  1400  C,  being  small  in  quantity,  were 
mixed,  and  5  cc.  agitated  with  20  cc.  of  water  but  2  cc.  remained 
undissolved.  The  aqueous  portion  likewise  gave  the  iodoform 
reaction. 
The  presence  of  acetone  in  the  bromoform  after  repeated  washing 
with  water  is  worthy  of  notice,  and  shows  the  necessity  of  frac- 
tionally redistilling  the  product.  Richter  [Organic  Chemistry, 
p.  161)  states  that  "  acetone  in  the  presence  of  caustic  soda  com- 
bines with  chloroform,  yielding  acetone  chloroform 
It  seems  not  unlikely  that  under  similar  conditions  a  correspond- 
ing compound  may  be  formed  with  bromoform. 
The  fraction  distilling  at  143 0  to  1480  C.  showed  a  sp.  gr.  of 
2-8645,  and  tnat  collected  at  148°  to  1 5 1 0  C.  had  a  gravity  of 
2-9082.  These  fractions  were  exposed  on  a  recent  cold  morning, 
and  at  9°-io°  began  to  cloud,  and  when  the  thermometer  marked 
8°  crystals  began  to  appear,  and  at  6°  C.  a  mass  of  crystals  had 
formed  in  each.  These  were  quickly  transferred  to  a  funnel,  a  small 
layer  of  absorbent  cotton  having  been  placed  in  the  angle  of  the 
funnel  and  the  liquid  portion  allowed  to  drain.  The  funnel  was  now 
brought  in-doors  and  the  crystals  allowed  to  melt,  the  first  portion 
that  escaped  from  the  funnel  was  collected  separately  and  the 
remainder  was  collected  in  a  perfectly  dry,  clean  vial,  and  is  believed 
to  be  chemically  pure  bromoform.  It  showed  the  following  charac- 
ters: specific  gravity  2-900  at  15°  C,  boiled  steadily  at  1470 
to  148°  C,  and  became  crystalline  at  6°  to  8°,  and  a  firm,  solid 
mass  at  —  4-5°  C.  These  temperatures  were  obtained  with  a  ther- 
mometer corrected  at  Yale.1 
The  lower  boiling  fractions  showed  no  signs  of  any  crystals  at 
The  liquid  remaining  in  the  flask  contains  considerable  calcium 
bromide.    An  attempt  was  made  to  recover  the  bromine  therein  as 
1  Since  writing  the  above,  Prof.  Maisch  has  called  my  attention  to  the  results 
reported  by  W.  H.  Perkin  in  Journal  of  the  Chemical  Society,  Proceedings, 
1884,  p.  533,  viz  :  spec.  grav.  2-90246  at  150  C. ;  melting-point  7-8°,  and  boiling- 
rjoint  120-3°  (pressure  330  mm.).  The  boiling-point  stated  is  evidently  a  mis- 
take, possibly  a  misprint. — G.  M.  B. 
(CH3)2c/ 
o°  C. 
