Into organic or inorganic the
incorporation of fluoroalkyl group substrates frequently results in materials
that have different properties like mechanical, biological as well as
biological, for a given application that are much more desirable than those of
the parent compound. Such as pyrimidine nucleosides the 5-trifluoromethyl are
known as inhibitor significantly tumor growth. By the reaction these species
are readily synthesized with appropriate halouracil derivatives along with the
organometallics compound.
For the syntheses the suitable
reagent is derivatives from the group IIB of organometallics compounds that
contain the perfluoroalkyl ligands.
The
mercurial, such as, halides of several group react with mercurial and form
compound like
using the
mercurial ligand exchange reaction, moreover, elevated temperature typically
required as well as the reaction time is long. Although
NMR approach
to the group of element in a basic solvents like pyridine the reaction had been
isolated no product formed.
Based on the observation that we
followed the procedure the compounds like methyl, trifluoromethyl, as well as
mixed methyl these sort of species are
present in the mixture that is formed when it react with the
Lewis base adduct is known as the compound
under vacuum
it does not undergo dissociation;
the isolation
as well as purification is readily accomplished.
Experiment of Bis (Trifluoromethyl) Cadmium 1, 2 Dimethoxymethane
By sublimation
is purified
at ambient temperature of
torr, to condense allowing the sublimate onto the
cooled surface to -10 degree. The successful synthesizes of
from the
thermal decarboxylation
these are
obtained at least twice prior the sublimed should be used. Over sodium
benzophenone ketyl as well as degassed Glyme 1, 2-dimethoxyethane is dried at
least two thaw cycles of freeze pump is used. From the reaction of the methyl
Grignard along with cadmium (II) Dimethyl cadmium could be prepared.
In a clean dry freshly sublimed
is placed
there in a 50mL round bottomed flask, and a stirring bar magnetic. With a
vacuum the flask is fitted stopcock to one end that affixed the joint 24/40; to
the other end of the stopcock an 18/9 ball joint is sealed. To a standard
vacuum line the flask is attached through the connection of ball-and-socket.
Into the reaction vessel approximately 10mL of purified Glyme is vacuum
distilled. From -196 degree as the substances of the flask are allowed to warm,
for several minutes they ought to be stirred magnetically certify the complete
dissolution
.
1.44g
has dissolved
the
, vacuum distillation during the reaction vessels.
For 2.3 hour the solution is stirred at ambient temperature. Slowly the
solution turned into cloudy during this time as to form the
. Under vacuum the volatile material is removed but
12 hour is required for this procedure and a white free flowing power is
remained behind the flask. Until the solid is thoroughly dry the content of the
vessels are then pumped as we described above the product is treated. The yield
is 57 percent.
Table: For Lewis base Adducts
NMR data
|
Chemical shift
(ppm)
|
|
|
44.1
|
448,471
|
|
46.7
|
354,374
|
|
44.5
|
457,476
|
Through two methods the Lewis
base adducts of
could be
easily synthesized. By utilizing THF a procedure analogous to the above is the
first method, pyridine (py) as well as the yield of different components are
50, 70 percent respectively. For the reaction to proceed the following
significant time is required. For 19 hour equilibrium THF used as a solvent.
Direct Lewis Base Exchange method is the other simplest method. When it
dissolved in the excess amount of pyridine gives the 96 percent yield.
Result & Discussion of Bis (Trifluoromethyl) Cadmium 1, 2 Dimethoxymethane
In ethers and haloalkanes the
compound
is soluble,
economically in arenes are soluble, as well as in alkanes insoluble. Under
the product
stored is best otherwise at low temperature Ar, meanwhile thermal
decomposition, 5% day, at ambient temperature. The first preparation of the
group 5A organometallics perfluoromethyl has grown steadily. Sophisticated
methodology is required for synthesizes of completely substituted compounds
such as reactors of metal atom discharge techniques, at elevated temperature
prolonged interaction of the reagents. Electropositive metals formation highly
substituted derivatives for example
with the only
reagent known to be effective through the ligand exchange reaction.
It is discussed that in a dry
Glyme from the excess of
as well as
CdMe2 BIS (trifluoromethyl) cadmium.glyme was best formed. Under
high vacuum by prolonged pumping after 3hour all volatile material is removed.
It soluble in the ethers as well as haloalkanes. At the end we get the yield of
95 to 96 percent. There is the following precaution that we should follow
during the experiments. As in an efficient hood the dimethyl cadmium is a
noxious smelling, toxic liquid that might be handled with the care.
It is
completely dry and might be spontaneously ignite in air. Under inert condition
all the times
could be
handled that is recommended (KRAUSE & MORRISO, 1980).
Conclusion of Bis (Trifluoromethyl) Cadmium 1, 2 Dimethoxymethane
It is concluded that with the help of the Bis
(Trifluoromethyl) Cadmium 1, 2 Dimethoxyethane we get the required solution of
.
By far the most convenient bis (trifluoromethyl) cadmium.glyme is known for the
preparation of trifluoromethyl substituted, under the ambient conditions the
reaction is required only some minutes. It is also concluded that we get the
yield 57, or 96 percent. Under further studies the mechanism of the reaction
along with the acyl halides, yet the fluorides quickly formed and at low
temperatures excellent yield is obtained. It also concluded that the in other
systems thermal generation of CF2 is required at much lower
temperature
is the clearly transfer reagent.
References of Bis (Trifluoromethyl) Cadmium 1, 2 Dimethoxymethane
[1]
|
L. J. KRAUSE and J.
A. MORRISO, "Bis( trifluoromethyl)cadmium*glyme (glyme =
dimethoxyethane), a New,Powerful Fluoroalkylating Agent and Low -temperature
Source ofDifluorocarbene," J.C.S. CHEM. COMM., 1980.
|