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Author Topic: Synthesis conventional of Sarin  (Read 491 times)

Basquyatti

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Synthesis conventional of Sarin
« on: October 02, 2018, 07:57:32 am »
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at room temperature and reacting with Hydrofluoric acid at low temperatures to form two phases, the upper phase is withdrawn and the lower one refluxed for the removal of the remaining hydrogen chloride, the material obtained is then brought to the third stage, where the DC obtained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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