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#Post#: 378--------------------------------------------------
The military preparation of FTH
By: Basquyatti Date: September 30, 2018, 11:04 pm
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FTH is prepared from the dissolution of phosphoryl trichloride
in solvent to react with dimethylamine at low temperatures to
prevent boiling of the reactants, crystallizing the solution,
sodium carbonate is added to dissolve the crystals and form
dimethylaminophosphoryl chloride (Nitron-2B), the insolubles are
filtered, the solvent distilled and the Nitron-2B distilled
under vacuum, this material obtained is then dissolved in
Chloroform and mixed with Ethanol and sodium fluoride and then
this is refluxed at 65 degrees Celsius, the precipitated
crystals are separated by addition of water for the dissolution
of sodium chloride, the product phase is in the lower phase and
is then extracted by separation funnel, the mixture is then
placed to distill for the removal of chloroform, the crystals of
FTH (FTHCl) are then dried outdoors or by vacuum filtration.
In a container add 156 grams of 98%~99% phosphoryl trichloride,
then add 500 milliliters of anhydrous 1,2-Dichloroethene or
Ethyl Ether, dissolve the agent at -5 degrees Celsius and when
dissolved add 46 grams of 98% liquid Dimethylamine, shake the
solution well and keep it below of -5° Celsius the reaction,
then crystallization of the solution, when crystallization or
crystallization is complete, add 107 grams of Sodium Carbonate
99% and leave the temperature to 0 degree Celsius and stir the
solution during the reaction. precipitates from the first
reaction will be dissolved and give room for a solid insoluble
powder sodium bicarbonate when all the insolubles of the first
reaction are dissolved, filter the solution, distill the solvent
at 40~60 degrees Celsius the solvent and then distil at 90
degrees Celsius in 22 mmHg the Nitron-2B. In a flask place
163.58 grams of Dimethylaminophosphoryl dichloride and add 610
milliliters of chloroform 99%, dissolve it in it and thereafter
add 46.53 grams of 99% Ethanol, keep the vessel under stirring
before adding the Ethanol, add the Ethanol, add 42.5 grams of
Sodium Fluoride 98%~99%, let the reaction take place on stirring
in the reflux apparatus at 65 degrees Celsius, keep this
reaction also on stirring, and more of two hours of reaction, a
very simple method of knowing that the reaction is over is no
longer the crystallization of Fluorotabun hydrochloride or
Hydrochloride. The sodium chloride is dissolved in 170
milliliters of distilled water at 20 degrees Celsius, the
solution is stirred for 5 minutes, then the water is filtered
with the salt, the solvent is distilled at 65 degrees Celsius
and the crystals are filtered through vacuum or let them air
dry.
#Post#: 379--------------------------------------------------
Re: The military preparation of FTH
By: zwclose7 Date: September 30, 2018, 11:08 pm
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Have you read A Laboratory History of Chemical Warfare Agents?
#Post#: 380--------------------------------------------------
Re: The military preparation of FTH
By: Basquyatti Date: October 1, 2018, 9:15 am
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Yes I read, the process is taken from the Preparatory Manual for
Chemical Warfare
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