Am'Zug.r;Sarm' }  Gleanings  from  the  German  Journals.  403 
it  is  not  necessary  to  use  the  expensive  commercial  articles.  In 
addition  to  the  method  of  Prof.  Spica,  it  is  possible  to  make  this 
new  compound  (1)  By  heating  in  a  steam-bath  the  molecular  pro- 
portions of  antipyrine  and  salicylic  acid  with  or  without  a  small 
quantity  of  water ;  after  cooling,  the  solid  mass  is  recrystallized 
from  alcohol;  (2)  The  antipyrine  is  dissolved  in  water,  the  salicylic 
acid  in  ether  ;  after  thorough  agitation  of  the  mixed  solutions  the 
salt  separates  out  slowly,  being  only  slightly  soluble  in  either 
liquid;  (3)  Very  pretty  crystals  can  be  obtained  by  dissolving  the 
antipyrine  in  chloroform,  the  salicylic  acid  in  ether  and  mixing  the 
two,  rather  dilute,  solutions.  The  salt  made  by  the  secret  method 
has  been  made  in  large  quantities,  and  the  results  of  its  use  in  hos- 
pitals have  been  very  favorable.  It  forms  a  coarsely  crystalline, 
white,  odorless  powder,  of  a  sweetish  not  unpleasant  taste ;  easily 
soluble  in  alcohol  and  benzol,  difficultly  soluble  in  ether  and  water 
(boiling  water,  4-4:100;  cold  water,  0-4:  100) ;  it  melts  at  91-5°  C. 
(Prof.  Spica,  89-900).  Sulphuric  acid  liberates  salicylic  acid  and 
sodium  hydrate  liberates  antipyrine,  allowing  an  easy  determina- 
tion of  purity.     A  weighed  quantity  is  dissolved  in  water  in  a 
■2 
separating  funnel,  a  measured  excess  of  —  sodium  hydrate  solution 
n 
added  and  the  separated  antipyrine  dissolved  by  agitating  with 
chloroform  ;  the  chloroform  solution  is  evaporated  in  a  tared  vessel, 
the  antipyrine  (42*3  per  cent.)  weighed  and  its  purity  further  estab- 
lished by  a  melting  point  determination  (should  be  1130).  The 
sodium  salicylate  solution  is  next  titrated  with  sulphuric  acid  and  the 
salicylic  acid  (577  per  cent.)  taken  up  with  ether,  the  ethereal  solu- 
tion evaporated  and  a  melting  point  determination  made  (should 
melt  at  1550  C). — Dr.  L.  Scholvien,  Pharm.  Ztg.s  1890,  395. 
Potassium  nitrate  in  potassium  iodide  is  positively  detected  by  the 
following  test:  By  use  of  pure  dilute  hydrochloric  acid  and  pure 
zinc  an  energetic  evolution  of  hydrogen  is  started,  after  8-10  min- 
utes the  solution  of  potassium  iodide,  to  which  some  starch  paste 
has  been  added,  is  introduced  ;  no  violet  or  blue  color  should  be 
produced  even  after  standing  some  time.  The  object  in  letting  the 
hydrogen  evolution  proceed  for  some  time  before  adding  the  potas- 
sium iodide  is  to  change  any  free  chlorine  which  may  be  present  in 
the  acid  into  hydrochloric  acid. — Dr.  Brenstein,  Pharm.  Ztg.,  1890, 
400. 
