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Chemistry / The military preparation of FTH
« Last post by Basquyatti on October 01, 2018, 12:04:27 pm »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.
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.
