﻿110 
  J. 
  G. 
  Spenzer 
  — 
  ft-Bromvalerianic 
  Acid. 
  

  

  The 
  non-magnetic 
  residue 
  of 
  the 
  above 
  analysis 
  contained 
  

   all 
  the 
  non-soluble 
  and 
  non-magnetic 
  residue 
  of 
  the 
  original 
  

   mass 
  treated, 
  together 
  with 
  all 
  the 
  dirt 
  accumulated 
  through- 
  

   out 
  the 
  long 
  process 
  of 
  treatment. 
  Nothing 
  of 
  interest 
  that 
  

   could 
  not 
  be 
  referred 
  with 
  almost 
  absolute 
  certainty 
  to 
  the 
  

   later 
  source 
  could 
  be 
  observed 
  in 
  it 
  in 
  a 
  careful 
  microscopic 
  

   examination. 
  Evidently 
  the 
  mass 
  treated 
  did 
  not 
  contain 
  

   diamonds 
  or 
  anything 
  remotely 
  suggestive 
  of 
  them. 
  

  

  Art. 
  X. 
  — 
  ft-Bromvalerianic 
  Acid, 
  CH^-CH^-CHBr- 
  

   CHi-COOH; 
  by 
  John 
  G. 
  Spenzer, 
  Cleveland, 
  O. 
  

  

  The 
  first 
  step 
  in 
  the 
  preparation 
  of 
  /9-brom 
  valerianic 
  acid 
  

   was 
  the 
  preparation 
  of 
  propylideneacetic 
  acids 
  by 
  the 
  action 
  

   of 
  hot, 
  caustic 
  soda 
  solution 
  on 
  ethylidene 
  propionic 
  acid. 
  

  

  To 
  one 
  volume 
  of 
  pure 
  propylideneacetic 
  acid 
  contained 
  in 
  

   a 
  small 
  cylinder 
  having 
  a 
  well 
  ground 
  stopper, 
  \\ 
  volumes 
  of 
  

   hydrobromic 
  acid 
  saturated 
  at 
  0° 
  C. 
  were 
  added, 
  on 
  shaking 
  a 
  

   clear 
  solution 
  resulted, 
  it 
  was 
  allowed 
  to 
  remain 
  quietly 
  for 
  24 
  

   hours 
  at 
  the 
  ordinary 
  temperature 
  ; 
  the 
  monobromide 
  had 
  now 
  

   risen 
  to 
  the 
  surface 
  of 
  the 
  hydrobromic 
  acid 
  as 
  a 
  light 
  brown 
  

   colored 
  layer. 
  The 
  cylinder 
  was 
  now 
  vigorously 
  shaken 
  from 
  

   time 
  to 
  time, 
  to 
  bring 
  any 
  unaltered 
  propylideneacetic 
  acid, 
  

   which 
  might 
  be 
  dissolved 
  in 
  the 
  monobromide 
  into 
  intimate 
  

   contact 
  with 
  the 
  hydrobromic 
  acid. 
  After 
  this 
  occasional 
  

   shaking 
  had 
  been 
  continued 
  for 
  four 
  or 
  five 
  days, 
  the 
  contents 
  

   of 
  the 
  cylinder 
  formed 
  two 
  distinct 
  layers, 
  the 
  reaction 
  was 
  

   ended 
  and 
  all 
  the 
  propylideneacetic 
  acid 
  had 
  been 
  quantita- 
  

   tively 
  changed 
  into 
  ^-bromvalerianic 
  acid. 
  The 
  cylinder 
  still 
  

   stoppered 
  was 
  now 
  placed 
  in 
  ice 
  water, 
  to 
  cause 
  the 
  new 
  acid 
  

   to 
  solidify, 
  this, 
  however, 
  did 
  not 
  occur 
  ; 
  it 
  was 
  then 
  placed 
  in 
  

   a 
  freezing 
  mixture 
  of 
  ice 
  and 
  salt, 
  and 
  on 
  agitating 
  slightly 
  the 
  

   monobromide 
  at 
  once 
  congealed 
  to 
  a 
  solid 
  mass 
  of 
  fine 
  needles 
  

   lying 
  on 
  the 
  surface 
  of 
  the 
  hydrobromic 
  acid. 
  The 
  cylinder 
  

   stood 
  for 
  15 
  hours 
  at 
  a 
  temperature 
  of 
  15° 
  C. 
  ; 
  then 
  the 
  crys- 
  

   talline 
  cake 
  was 
  broken 
  through 
  with 
  a 
  glass 
  rod, 
  distributed 
  

   through 
  the 
  hydrobromic 
  acid 
  and 
  brought 
  into 
  a 
  platinum 
  

   cone, 
  where 
  it 
  was 
  allowed 
  to 
  dry, 
  being 
  washed 
  with 
  small 
  

   successive 
  portions 
  of 
  ice 
  water, 
  in 
  order 
  to 
  remove 
  the 
  greater 
  

   part 
  of 
  the 
  mineral 
  acid. 
  

  

  The 
  contents 
  of 
  the 
  cone 
  were 
  now 
  brought 
  on 
  to 
  a 
  watch 
  

   glass 
  and 
  placed 
  in 
  a 
  vacuum 
  over 
  sulphuric 
  acid 
  and 
  caustic 
  

   potassa; 
  a 
  dry 
  sandy, 
  white 
  substance 
  resulted, 
  which 
  was 
  pow- 
  

   dered 
  and 
  recrystallized 
  out 
  of 
  petroleum 
  ether. 
  So 
  produced, 
  

   the 
  /3-bromvalerianic 
  acid 
  is, 
  after 
  drying, 
  perfectly 
  pure, 
  as 
  the 
  

   analysis 
  proves 
  : 
  

  

  