FREE BOOKS

Author's List




PREV.   NEXT  
|<   72   73   74   75   76   77   78   79   80   81   82   83   84   85   86   87   88   89   90   91   92   93   94   95   96  
97   98   99   100   101   102   103   104   105   106   107   108   109   110   111   112   113   114   115   116   117   118   119   120   121   >>   >|  
lour after standing for a few hours. Hence, the observations should be confirmed by isolation of the crystals of brommethylfurfural. No trace of this substance is obtained from the xylose product. In order to identify the substance, the ether extract, after neutralisation, is allowed to evaporate to a syrup, and crystallisation promoted either by rubbing with a glass rod, or by the more certain and highly characteristic method of 'sowing' with the most minute trace of omega-brommethylfurfural, when crystals are almost instantly formed. These are recrystallised from ether, or a mixture of ether and light petroleum, and further identified by the melting-point (59.5-60.5 deg.), and, if considered desirable, by estimation of the bromine. It is now found, so reactive is the bromine atom in this compound, that the estimation may be accurately made by titration with silver nitrate according to Volhard's process, the crystals for this purpose being dissolved in dilute alcohol: 0.1970 gram required 10.5 c.c. _N_/10 AgNO_{3}. Br = 42.63 p.ct., calculated 42.32 p.ct. This method of applying hydrogen bromide in ethereal solution is, of course, unsuitable for investigations where a higher temperature has to be employed, or where long standing is necessary, since, under such circumstances, the ether itself is attacked. Wishing to make investigations under these conditions, the authors have tried several solvents, and, at present, find that chloroform is best suited to the purpose. In each of the following experiments, 10 grms. of the substance were covered with 250 c.c. of chloroform which had been saturated at 0 deg. with dry hydrogen bromide. The mixture was contained in an accurately stoppered bottle, firmly secured with an iron clamp, and heated in a water-bath to about the boiling temperature for two hours. After standing for several hours, the mixture was treated with sodium carbonate (first anhydrous solid, and afterwards a few drops of strong solution), filtered, and the solution dried over calcium chloride. Most of the chloroform was then distilled off, and the remaining solution allowed to evaporate to a thick syrup in a weighed dish. The product was then tested for omega-brommethylfurfural by 'sowing' with the most minute trace of the substance, as described above. It was then warmed on a water-oven, kept in a vacuum desiccator over solid paraffin, and the weight estimated. When necessary, the product was recrys
PREV.   NEXT  
|<   72   73   74   75   76   77   78   79   80   81   82   83   84   85   86   87   88   89   90   91   92   93   94   95   96  
97   98   99   100   101   102   103   104   105   106   107   108   109   110   111   112   113   114   115   116   117   118   119   120   121   >>   >|  



Top keywords:

solution

 

substance

 

product

 

mixture

 

standing

 

chloroform

 
brommethylfurfural
 

crystals

 

sowing

 

method


estimation

 

bromine

 
minute
 

evaporate

 

temperature

 

accurately

 

investigations

 
bromide
 
hydrogen
 

purpose


allowed

 
contained
 

saturated

 
present
 
authors
 

conditions

 

Wishing

 

solvents

 
experiments
 

suited


covered

 

tested

 

weighed

 

distilled

 

remaining

 

warmed

 

weight

 

estimated

 

recrys

 
paraffin

desiccator

 
vacuum
 

chloride

 

calcium

 
boiling
 

heated

 

bottle

 

firmly

 
secured
 

treated