88 M. C, Lea on Nitrate of Ethyl. 
be found in small quantities and lead, when the crude contents 
of the pressure tubes are first distilled with caustic alkali, to the 
formation of a substance analogous to Boutlerow’s methylenitane 
in the ethyl! series. 
Further remarks on the preparation of the Ethyl bases by means of Nitrate 
of Ethyl, and their separation. 
Frequent repetition of the process which I have previously 
described* confirms me in my opinion of its advantages. Nitrate 
of ethyl is obtained easily and abundantly. From 480 grammes of 
alcohol of 40° Baumé, I have obtained 231 of nitrate of ethyl, and 
even a still larger proportion. It is essential in operating upon 
quantities of half a litre or over, of the mixture of alcohol and © 
nitric acid to first raise the alcohol to a boiling heat and dissolve 
the urea in it, and then add the nitric acid, otherwise it may 
attack the alcohol while the urea remains undissolved at the bot- 
tom of the vessel, and thus cause the whole process to fail. | 
have prepared six or seven pounds of nitrate of ethyl in this way 
with very little trouble. 
In acting upon the nitrate of ethyl with ammonia, it is neces 
sary that the pressure tubes should be extremely strong and 
should never be more than one-half full. Saline baths are not 
to be used. ; 
Triethylamine appears to be only an occasional product of this 
reaction. . 
In employing the process which I have recommended for 
removing the ammonia, viz: converting the mixed bases into 
sulphates and exhausting with absolute alcohol, it does not 
answer well to add sulphuric acid to the crude products obtained 
from the pressure tubes, because it is impossible to know the 
exact quantity of sulphuric acid required to expel the nitric acid. 
If too little be employed, some titrate of ammonia might remail 
and dissolve in the alcohol. If too much, bisulphate of ammonia 
may be formed, and this likewise would dissolve to some extent 
in the alcohol and contaminate the product. It is therefore n& 
cessary to distil the crude products with caustic alkali, neutral- 
ize exactly with SO, and then evaporate to dryness and exhaust 
with alcohol as described in the paper here referred to. 
In employing picric acid to ae the ethyl bases, each 
picrate, after having been purified by recrystallizations, is to » 
treated with chlorhydric acid. The greater part of the pieri¢ 
id separates, and a further portion by evaporating the liquid. 
Some however remains, and it is important to get md of it, be: 
cause picric acid when distilled with aqueous caustic alk 
evolves ammonia, which would thus contaminate the ethy] bas¢ 
* This Journal, July, 1861, 
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