224  ON  THE  PRODUCTION  OF  NITRATE  OF  METHYL. 
vitriol.  Judging  from  the  reactions  of  ethylic  alcohol,  it  did 
not  appear  to  me  probable  that  such  a  proceeding  could  succeed. 
It  was  tried,  however,  and  with  the  following  results. 
The  substances  were  placed  in  a  flask  capable  of  containing 
twenty  times  their  united  volume,  which  was  connected  with  a 
Liebig's  condenser  by  a  wide  delivery  tube.  For  a  few  minutes 
no  action  was  perceptible,  but  it  soon  set  in,  with  rapidly  in- 
creasing violence.  Torrents  of  gaseous  products  with  deep  red 
fumes  of  oxydes  of  nitrogen,  were  evolved,  and  presently  the  ap- 
paratus blew  up  with  a  loud  explosion,  and  had  not  due  precau- 
tion been  taken  with  a  view  to  a  possible  unpleasant  conclusion, 
personal  inconvenience  might  have  resulted,  for  the  3-litre  flask 
was  shattered  into  very  small  pieces,  which  were  thrown  to  a 
considerable  distance.  The  quantities  operated  upon,  were  small, 
50  grammes  of  methylic  alcohol  and  proportionate  quantities  of 
the  other  substances.    No  heat  was  applied. 
It  is  scarcely  probable  that  the  gases  were  evolved  in  such 
quantities  as  to  have  caused  the  explosion.  It  seems  more 
likely  that  the  heat  generated  by  the  reaction  was  sufficient  to 
raise  the  temperature  of  the  interior  of  the  flask  to  1509  C,  at 
or  below  which  point,  according  to  Dumas,  the  vapor  of  methylic 
nitrate  explodes. 
I  have  had  no  difficulty,  however,  in  preparing  this  ether  by 
a  different  process.  By  dissolving  a  considerable  quantity  of 
urea  or  nitrate  of  urea  in  methylic  alcohol,  it  supports  the  action 
of  nitric  acid  with  the  utmost  facility.  The  following  are  the 
proportions  which  I  have  employed. 
Into  a  retort  of  the  capacity  of  a  litre,  200  c.  c.  of  purified 
wood  spirit  are  placed,  and  about  40  grammes  of  nitrate  of 
urea  are  added  and  heat  applied.  When  solution  has  nearly 
taken  place,  150  c.  c.  of  nitric  acid  free  from  the  lower  oxydes 
of  nitrogen,*  sp.  gr.  1-31,  are  added,  and  the  mixture  is  distilled 
to  one-third.  170  c.  c.  of  wood  spirit  and  130  of  nitric  acid  are 
then  added  and  distilled  to  the  same  point.    Finally,  150  c.  c. 
*  Freedom  from  the  lower  oxydes  is  an  essential  condition  of  success. 
That  nitric  acid  is  colorless  is  not  in  itself  a  sufficient  indication  of  purity 
in  this  respect.  An  acid  which  causes  the  least  darkening  to  a  solution 
of  ferrous  sulphate  is  wholly  unfit  for  use  in  the  preparation  of  either 
methylic  or  ethylic  nitrate. 
