SCG 
THE PHARMACEUTICAL JOURNAL AND TRANSACTIONS. 
[April 29, 1871. 
and a moderate heat is applied and very gradually in¬ 
creased. As soon as the mixture approaches boiling, the 
fire is removed and the reaction allowed to continue. If 
the application of the heat has been too rapid or too long 
continued, considerable frothing occurs and the contents 
of the retort are apt to foam over. With a moderate and 
slowly increased heat the reaction is less violent, and the 
temperature rises gradually after the removal of the fire 
and the beginning of boiling. As soon as the thermo¬ 
meter, inserted into the tub ulus, rises above 100° C. 
(212° F.) the receiver is changed, the distillate now be¬ 
coming more and more mixed with ethyl-amylic ether 
and nitrate of amyl, readily perceived by the change in 
odour. 
The distillate obtained below 100° C. is now agitated 
with an aqueous solution of caustic or carbonate of po¬ 
tash, to remove free acids, and after separation the oily 
liquid is introduced into a clean retort and again slowly 
heated. The first portion coming over contains the 
amylic aldehyde. When the very slowly increased heat 
has risen to 96° C., the receiver is again changed and the 
distillate now collected as nitrite of amyl, until the 
thermometer reaches 100° C., when the distillation is 
stopped. 
It will be observed that the process for the preparation 
of this compound consists of two distinct operations; 
first, the production of the amyl-nitrous ether, and, se¬ 
condly, its purification. In both operations the very 
gradual application and increase of heat is very essential. 
The yield, is small; not having kept any record of the 
yield, I am unable to give the percentage obtained. All 
the amylo-nitrous ether dispensed by me was made by 
this process. 
After the publication of Redwood’s process for spirit 
of nitrous ether, * it was repeatedly tried with entirely 
satisfactory results, and the idea naturally suggested 
itself to apply the same process to the similar com¬ 
pound amylo-nitrous ether. Accordingly, amylic al¬ 
cohol was mixed with sulphuric acid, the mixture in¬ 
troduced into a retort together with some copper wire, 
and, after cooling, nitric acid was added. In a very few 
moments the evolution of gas was observed, the liquid 
became hot without the external application of heat, and 
the reaction very rapidly increased to such a violence 
that the entire charge was lost, it being impossible to 
condense any vapours in a Liebig’s condenser, or to re¬ 
tain much of the liquid forced over, in the receiver. The 
experiment was never repeated. 
Nadlerf gives a process which he says readily yields 
the pure nitrite. It having come but lately under my 
notice, I am not prepared to speak about its merits ; it 
consists in distilling amylo-sulphate of potash with 
nitrate of potash. 
The composition of the nitrite of oxide of amyl is 
CioIInO, N0 3 ; it ‘appears to me that we ought to dis¬ 
continue this long name, as well as also nitrite of amyl. 
Amylo-nitrous ether expresses the chemical relations of 
this compound, and the similarity of names also indi¬ 
cates its analogy to the officinal ethylo-nitrous ether, 
which may well be continued to be called nitrous ether, 
just as ethylic alcohol and all its direct derivatives 
are called by their generic names merely—alcohol, alde¬ 
hyde, ether—without any prefix .—American Journal of 
Pharmacy. 
NEUTRAL CRYSTALLIZABLE PRINCIPLE IN BLACK 
SNAKE ROOT (CIMICIFUGA ACEMOSA). 
BY T. ELLWOOD CONARD. 
As tins plant is a very common one, and has been fully 
described in articles heretofore written, I will not enter 
into any description of it, but, merely state the condition 
of the root acted upon; and of the very many experi¬ 
* See Amer. Journ. Pharm. 1867, p. 330. 
f Ann. Chem. und Pharm. vol. cxvi. p. 176. 
ments made I will give those only which resulted most 
satisfactorily. 
In order to get the advantage, if there should be any, 
in using the perfectly fresh root, I obtained it in this 
way directly from the ground. It was dug in the latter 
part of July, at which time the roots were quite well 
developed. 
A portion of these, thoroughly cut and bruised, were 
put in a still with water, and a varied and continued 
heat was applied, but without producing in the distillate 
any preceptible amount of volatile principle. The addi¬ 
tion of liquor potass® to the mixture and redistillation 
was tried, which also failed to develope a volatile oil or 
other substance ; there was no separation of anything 
from the water which distilled over, nor had it any taste 
or smell, except an earthy, rooty taste, characteristic of 
any inert vegetable matter. From these facts we infer 
the root does not owe its active properties to the posses¬ 
sion of a volatile substance. 
The next experiments I will give in outline. Three 
and a half pounds of the root, cut and bruised, were 
treated with four and a half pints of strong alcohol by 
maceration for four weeks and filtered. Two pints of 
this tincture was treated with three fluid ounces of the 
solution of subacetate of lead, which completely precipi¬ 
tated the resin, tannin, etc. and most of the colouring- 
matter, as will be seen below. The lead was separated 
from the filtered liquid by means of sulphuretted hydrogen 
in excess; after agitating for some time together, filtered. 
A repetition of the process proved the solution to be en¬ 
tirely free from resinous or gummy substances, also from 
much colouring matter. The tincture was set aside and 
allowed to evaporate spontaneously. The resulting 
powder was treated repeatedly with benzine. The 
several washings were mixed and evaporated, yielding a 
minute portion of a disagreeable nauseous, fatty sub¬ 
stance without colour. The ‘powder was freed from the 
odour of benzine, placed on a filter and thoroughly 
washed with water ; then dried and dissolved in sixteen 
times its weight of strong alcohol, forming a saturated 
solution. This was mixed with one hundred and twenty 
grains of pure alumina, moistened with a few drops of 
water, and agitated for twenty-four hours, then put in 
a capsule and evaporated spontaneously to a very dry 
light mass. This was put on a filter, and hot alcohol 
poured on it until entirely exhausted. This was allowed 
to evaporate, and there remained a crystalline substance 
of a light yellow colour, not of a very regular or decided 
shape, but of a massy appearance, resembling almost 
exactly the crystals of sulphate of alumina on a small 
scale. But under the microscope, at a low power, their 
crystalline form was more distinct, presenting an appear¬ 
ance similar to that of rock candy. This substance, in 
powder, has little taste, on account of its extreme insolu¬ 
bility in the liquids of the mouth. But its solution in 
alcohol has the intensely acrid and sharp taste that cha¬ 
racterizes recent cimicifuga. 
The crystals have the following characteristics:—They 
are very soluble in cold alcohol, more so when heated. 
Dissolve readily in dilute alcohol, also in chloroform, and 
slightly in ether; but are entirely insoluble in benzine, 
turpentine and bisulphide of carbon. Fusible at a mo¬ 
derate temperature, at a higher taking fire, and at a 
red heat entirely dissipated. 
This substance, from the following experiments and 
their results, appears to be a neutral principle :— 
A small quantity moistened on a jar lid with liquor 
potass®, and approached with the stopper of a muriatic 
acid bottle, did not give off the characteristic white fumes 
of a volatile alkaloid, nor did it produce fumes when 
heated with liquor potass® and brought near muriatic 
acid, as an ordinary alkaloid. A small quantity with 
liquor potass® put in a tube with a small outlet, was 
gently heated, but no odour of ammonia was given ofl. 
Reddened litmus paper remains imehanged by continued 
contact with its solution. Entirely incompatible with 
