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#Post#: 383--------------------------------------------------
Synthesis conventional of Sarin
By: Basquyatti Date: October 1, 2018, 6:57 pm
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Sarin is obtained in three steps, the first step is to produce
methylphosphoryl dichloride (DC), DC is obtained by
Kinnear-Perren reaction, which consists of using a mixture of
one mole of phosphorus trichloride to be mixed with one mole of
Aluminum trichloride at room temperature, then this mixture is
placed in a freezer-filled vessel to react with an atmosphere of
one mole of Chloromethane to give a mole of insoluble complex of
ionic character with a melting point ranging from 275 degrees
Celsius to 280 degrees Celsius, this complex is then filtered,
weighed and dried to be dissolved in Dichloromethane and
hydrolyzed in 36% hydrochloric acid, Hydrogen chloride serves to
prevent the decomposition of DC, the reaction forms two phases
in which are constituted by a higher acid water phase and a
lower phase consisting of aluminum trichloride hexahydrated
crystals, and a solution of DC and dichloromethane, the mixture
is then separated by a separatory funnel, the insolubles
filtered, the solvent distilled and the DC vacuum distilled to
be purified, stored and prepared for the second step, the second
step consists of dissolving a mole of DC in dichloromethane at
room temperature and reacting with Hydrofluoric acid at low
temperatures to form two phases, the upper phase is withdrawn
and the lower one refluxed for the removal of the remaining
hydrogen chloride, the material obtained is then brought to the
third stage, where the DC obtained in the first step is added,
adding Dichloromethane is used for the dissolution of more
products and Isopropanol is added to the solution, the mixture
is kept at room temperature (25 degrees Celsius) and then
refluxed until all hydrogen chloride is emitted, the solvent is
distilled and the Sarin distilled under vacuum. Note: Sarin and
Dichloromethane may already be used for military stock or direct
military operations, the mixture of Dichloromethane and Sarin
tends to persist about 2X higher because the mixture is
insoluble in water and not reactive in it.
Reaction GB (Di-Di, Hydrofluoric Acid)
Step 1. Preparation of methylphosphoryl Dichloride.
Using 138.72 grams of phosphorus trichloride 99%, place it in a
pressure-suppressing apparatus and add 134.68 grams of anhydrous
aluminum trichloride, stir the solution for 30 minutes at room
temperature, after 30 minutes close the vessel, cool it to 0
degrees Celsius or below and introduce 51 grams of anhydrous
Chloromethane, stir for 1 hour while introducing the agent and
then let it react under pressure until there is no more in the
vessel and the solution has completely crystallized, the end of
the reaction is around 36 to 48 hours, filter the crystals and
allow them to air dry or vacuum. Use 325 grams of crystals
obtained from the first step to be placed in an open vessel, add
171.6 grams of Dichloromethane 99% into the vessel where the
crystals are contained, begin stirring the mixture, stir the
solution for 30 minutes and lower the temperature of the mixture
to 0 degrees Celsius, after the time, add 305 ml of Hydrochloric
Acid 36%, keeping the temperature at 0 degree Celsius and on
vigorous agitation until it does not form more insoluble in the
bottom of the container, see in times the formation of water and
emission of Hydrogen Chloride, finished the formation of the
upper phase with acidic water and there is no more the emission
of Hydrogen Chloride, stop stir the mixture and bring the
solution to a separatory funnel, stir the mixture a little to
form the phase, leaving an exhaust outlet, forming the phases,
remove the the lower phase where the DC is contained, then take
the DC to filter and onwards, bring the mixture of DC and
Dichloromethane to a Distillation Apparatus and distill
Dichloromethane at 40 degrees Celsius and soon thereafter vacuum
the DC of 75 degrees Celsius at 24 mmHg, the material obtained
is a semi-solid mass at a temperature of 25 degrees Celsius.
Stock the DC for the second step.
Step 2. Preparation of methylphosphoryl Difluoride (DF or
Difluoro).
Take the DC product obtained from the first step and remove
67.81 grams from it and place in a vessel that is not attacked
by Hydrofluoric Acid, shortly thereafter add 171.6 milliliters
of Dichloromethane 99%, shake the mixture for 10 minutes and
then then add 41.6875 grams of 48% hydrofluoric acid, cool the
solution temperature to 0 degrees Celsius and start shaking it
until no more hydrogen chloride is emitted, the emission is
finished, stop shaking the solution, bring the solution to a
separatory funnel, let two phases form in the solution and
remove the product contained in the lower part, take the part
removed and place it in a reflux apparatus and let reflux for
the withdrawal of hydrogen chloride at cold reflux (-10 degree
Celsius ) of 70 degrees Celsius. Finished the remaining emission
of Hydrogen Chloride stops the reflux and leaves the material
stocked in Teflon containers next to Dichloromethane until its
use in the last step.
Step 3. Preparation of Sarin.
Take the material obtained, mixed with Dichloromethane and mix
with the other 67.81 grams of DC and add 85.8 grams of
Dichloromethane 99% therein, start shaking for 10 minutes at
room temperature, add 60.1 milliliters of Isopropanol 99 , 98%,
start shaking again for almost half an hour at room temperature,
transfer the vessel to a cold (-10 degree Celsius) reflux
apparatus, start stirring the mixture again and heat the
solution to 75 degrees Celsius, stop heating until all hydrogen
gas is emitted, or after 60 minutes. After the time has passed
and there is no further emission of hydrogen chloride from the
solution and there is no longer the formation of insolubles,
stop the reflux, leave the solution temperature in the
environment, filter the insolubles, distill the solvent at 40
degrees Celsius and then distill Sarin vacuum at 60 degree
Celsius at 15 mmHg.
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