Preparation of Hypophosphorus AcidP

Preparation of Hypophosphorus Acid

Preparation of Sodium Hypophosphite (Brit. Pat. 803179)

115g of white phosphorous is emulsified and reacted with aqueous NaOH to obtain 270g NaH2PO2.H2O (70%).

Preparation of aqueous sodium hypophosphite (Jap. Pat. 58185412)

White phosphorus is dispersed together with slaked lime used as an assistant in an aqueous medium by stirring in an inert gas atmosphere under heating at or above the melting point of white phosphorus. The dispersion is mixed with a solution of caustic soda under heating and stirring to effect the reaction of the components. The product is separated into solid and liquid, and the mother liquor is added with a phosphate donor such as phosphoric acid. When the phosphate donor is phosphoric acid, its amount is about 0.6mol per 1mol of dissolved calcium, and the pH of the system is maintained usually to about 8-11. The reaction is carried out at about 50-100°C, and the reaction product is aged for about 30min. The Ca(II) dissolved in the mother liquid is precipitated in the form of calcium apatite, and the high-purity aqueous solution of sodium hypophosphite can be recovered by this process.

Hypophosphorous acid purification

Free hypophosphorous acid, H3PO2, is prepared by acidifying aqueous solutions of hypophosphite ions, H2PO2-. For example, the solution remaining when phosphine is prepared from the reaction of white phosphorus and a base contains the H2PO2- ion. If barium hydroxide, Ba(OH)2, is used as the base and the solution is acidified with sulfuric acid, barium sulfate, precipitates and an aqueous solution of hypophosphorous acid results.

Ba2+ + 2 H2PO2- + 2 H3O+ + SO42- => BaSO4 + 2 H3PO2 + 2 H2O

The pure acid cannot be isolated merely by evaporating the water, however, because of the easy oxidation of the hypophosphorous acid to phosphoric acids (and elemental phosphorus) and its disproportionation to phosphine and phosphorous acid. The pure acid can be obtained by extraction of its aqueous solution by diethyl ether. Pure hypophosphorous acid forms white crystals that melt at 26.5° C. The electronic structure of hypophosphorous acid is such that it has only one hydrogen atom bound to oxygen, and thus it is a monoprotic oxyacid. It is a weak acid and forms only one series of salts, the hypophosphites. Hydrated sodium hypophosphite, NaH2PO2×H2O, is used as an industrial reducing agent, particularly for the electroless plating of nickel onto metals and nonmetals.

Hypophosphorous acid from sodium hypophosphite

To a stirred solution of 717.8 g of a 32% hydrochloric acid solution in a 3-necked 2 liter flask was added 615.42 g of powdered sodium hypophosphite. The temperature of the solution rose about 2° C. Water was removed from the stirred reaction mixture by reduced pressure distillation at a temperature of about 55°C ±7° C at a pressure of 44-72 mmHg until a hypophosphorous acid concentration of about 80 wt% was obtained. After cooling to room temperature, sodium chloride that had precipitated was filtered from the reaction mixture. The filter cake was washed twice with 32 wt % hydrochloric acid.

The recovered product contained 355.7 g of hypophosphorous acid. The analysis showed that the product contained 0.9 wt% sodium, 3.2 wt% chloride, and 80.96 wt% hypophosphorus acid. Chloride ion was removed from hypophosphorous acid using an ion-exchange column (height 221/4", diameter 11/8"). The column was packed with Rohm and Haas Resin IRA-410 in the chloride form and was regenerated using 5% NaOH.

The results from using this column at different H3PO2 and Cl- concentrations are shown below.
Influent Composition

Effluent Composition

H3PO2 %

Chloride %
46

3.0

49.6

0.06
46

3.0

46.7

0.09
71

5.9

52.6

0.02


Ephedrine Reduction to Methamphetamine with Hypophosphorus Acid and Iodine

By Wizard X

I would recommend a large excess of reducing agent for quick reduction. Charge flask with 100 ml (0.1Lt) of 50% H3PO2 (0.965 mole H3PO2 per 100 ml) fit reflux condenser, add 3x33 grams (99 grams, 0.39 mole) portions of I2 while cooling in ice bath down the reflux condenser[1]. After addition of I2, gently heat so HI gas is evolving from the condenser, add 5 mls potions of H2O down the condenser till HI gas stops evolving and hence maximum amount of HI saturation kept in solution is acheived. Now add 50.4 g (0.25 mole) of ephedrine hydrochloride and boil under reflux for at least 2 hours, let cool and then made basic with 20 % sodium hydroxide solution (20 grams NaOH in 100 mls H2O) in ice bath to liberate the free base. Set-up glassware for steam distillation and steam distil until the distillate is almost neutral to litmus.[2]

The libertated freebase methamphetamine which seperates is solvent extracted with three, 50-75 ml ether (or toluene) portions and the ether/amine solution is first washed with 50 mls of distilled water and the ether/amine solution dried with anhydrous sodium carbonate.[3] After removal of the ether (or toluene), the oil was vacuum distilled at a vacuum of 15 mmHg at 93°C. The yield is 80 - 82%[4].

Notes:

If I2 sticks to the condenser wall, wash down with distilled water.
Have the distillate receiving flask in ice. And cool down to 4-5 degC.
Anhydrous magnesium sulphate can be used. Rinse the anhydrous magnesium sulphate with a little ether (or toluene) after drying the main ether/amine solution.

Ephedrine Reduction

Major reduction reaction:

C6H5-(CHOH)-CH(NHCH3)-CH3 + HI =====> C6H5-(CHI)-CH(NHCH3)-CH3 + H2O

C6H5-(CHI)-CH(NHCH3)-CH3 + HI =====> C6H5-CH2-CH(NHCH3)-CH3 + I2

Minor reduction reaction:

C6H5-(CHI)-CH(NHCH3)-CH3 + H3PO2 + H2O =====> C6H5-CH2-CH(NHCH3)-CH3 + H3PO3 + HI

Ratio of ephedrine to HI is theoretically 1:2, however a 1:3 is used for better reduction and yeild.
Hypophosphorus to HI Calculations

H3PO2 + H2O + I2 ==>> H3PO3 + 2HI

Hypophosphorous 50% w/w. F.W = 66 g/mol. Density = 1.274 g/ml.

100mls (0.1Lt) of Hypophosphorous 50% w/w contains:

(1.274 / 50)/100 = 0.637 g/ml H3PO2 = 0.00965 mol/ml H3PO2.

0.00965 mol/ml H3PO2 x 100 = 0.965 mol/100ml H3PO2.

OR

(0.637/66) x 1000 = 9.65 moles H3PO2 per 1000 mls. (mol/Lt)

Since we use 100mls (0.1Lt), then 9.65 x 0.1 = 0.965 mol/100ml H3PO2. Now since the ratio of Ephedrine : HI is 1:3 = (3/1), we require 0.75 moles of HI for every 0.25 moles of ephedrine hydrochloride. Since we have 0.965 mol of H3PO2 and 0.39 moles of I2 (99/253.8 = 0.39), then the ratio of I2:HI is 1:2 = (2/1); so 0.39 moles of I2 reacts with the Hypophosphorous acid to form 0.39 x 2 = 0.78 moles of HI.

Finally, the excess Hypophosphorous acid, H3PO2 is 0.965-0.39 = 0.575 moles of H3PO2 is excess. The ratio for H3PO2 : I2 is 1:1, so only 0.39 moles of H3PO2 is needed to react with 0.39 moles of I2 to form 0.78 moles of HI. Not only do we have enough HI; 0.78 moles to reduce 0.25 moles of ephedrine hydrochloride, but a large excess of 0.575 moles of H3PO2.

Alternatively, Charge a 1000ml flask with 100 ml (0.1Lt) of 50% H3PO2 (0.965 mole H3PO2 per 100 ml), 100 mls of distilled water, fit reflux condenser, add 4x49.5 grams (198 grams, 0.78 mole) portions of I2 while cooling in ice bath down the reflux condenser[1]. After addition of I2, gently heat so HI gas is evolving from the condenser, add 10 mls potions of H2O down the condenser till HI gas stops evolving and hence maximum amount of HI saturation kept in solution is acheived. Now add 100.8 g (0.5 mole) of ephedrine hydrochloride and boil under reflux for at least 2 hours, let cool and then made basic with 20 % sodium hydroxide solution (20 grams NaOH in 100 mls H2O) in ice bath to liberate the free base. Set-up glassware for steam distillation and steam distil until the distillate is almost neutral to litmus.[2]

Since we have 0.965 mol of H3PO2 and 0.78 moles of I2 (198/253.8 = 0.78), then the ratio of I2 : HI is 1: 2 = (2/1); so 0.78 moles of I2 reacts with the Hypophosphorous acid to form 0.78 x 2 = 1.56 moles of HI. Finally, the excess hypophosphorus acid, H3PO2 is 0.965-0.78 = 0.185 moles of H3PO2 is excess. The ratio for H3PO2 : I2 is 1:1, so only 0.78 moles of H3PO2 is needed to react with 0.78 moles of I2 to form 1.56 moles of HI. Not only do we have enough HI; 1.56 moles to reduce 0.5 moles of ephedrine hydrochloride, but an excess of 0.185 moles of H3PO2.
P-fed Reduction to Methamphetamine with Hypophosphorus Acid and Iodine

By Pebble

Assuming that you have extracted P-fed from your pills, you are now ready to convert the p-fed to methamphetamine. The structure of P-fed is so closly related to methamphetamine, that people have learned to alter it's structure in order to convert it to methamphetamine.

What one is actually doing is reducing a benzylic alcohol. In our case, it appears as OH in P-fed. So, we strip this off completly and throw on an additional H (Hydrogen) to the p-fed. So, by removing the OH and adding a H we have thus altered the structure and have created methamphetamine.

This is for small-scale reduction of P-fed to methamphetamine. If one wanted to make meth in the range of ounces, etc. I would not reccomend one cook in an open container. Fire or explosion are at a much higher risk when cooking anything above 10 grams using this procedure. This is why the Push/Pull apparatus is so popular. No, fumes, smell, and IT CAN reduce the risk of injury if something does go wrong. Notice I said IT CAN. There is no fool-proof method of safety when working with chemicals of this nature, unless proper lab equipment, etc are used; and this still does not elimanate the dangers, just reduces the probability that an accident will happen.

If one wanted to have 5 grams as their finished peoduct, than 6-8 grams of P-fed. Some can get 90% yield where others may only get 35% yield. This takes time to perfect, but results will vary WITH YOU.

Take your 8 grams of p-fed and put this into a 250ml. flask or pyrex meassuring cup. Slowing add Iodine crystals unto the p-fed is mixed well with the

النتائج (الإنجليزية) 2:

Preparation of Hypophosphorus Acid Preparation of Sodium Hypophosphite (Brit. Pat. 803,179) 115 g of white phosphorous is emulsified and reacted with 270 g Aqueous NaOH to Obtain NaH2PO2.H2O (70%). Preparation of Aqueous Sodium hypophosphite (Jap. Pat. 58185412) White phosphorus is dispersed together with slaked lime used as an assistant in an aqueous medium by stirring in an inert gas atmosphere under heating at or above the melting point of white phosphorus. The dispersion is mixed with a solution of caustic soda under heating and stirring to effect the reaction of the components. The product is separated into solid and liquid, and the mother liquor is added with a phosphate donor such as phosphoric acid. When the phosphate donor is phosphoric acid, its amount is about 0.6mol per 1mol of dissolved calcium, and the pH of the system is maintained usually to about 8-11. The reaction is carried out at about 50-100 ° C, and the reaction product is aged for about 30min. The Ca (II) dissolved in the mother liquid is precipitated Calcium in the form of apatite, and the High-Purity Aqueous Solution of Sodium hypophosphite CAN be Recovered by this Process. Hypophosphorous acid Purification Free Hypophosphorous acid, H3PO2, is Prepared by acidifying Aqueous solutions of hypophosphite ions, H2PO2-. For Example, the solution remaining when phosphine is prepared from the reaction of white phosphorus and a base contains the H2PO2- ion. If barium hydroxide, Ba (OH) 2, is used as the base and the solution is acidified with sulfuric acid, barium sulfate, precipitates and an Aqueous Solution of Hypophosphorous acid results. Ba2 + + 2 H2PO2- + 2 H3O + + SO42- => BaSO4 + 2 H3PO2 + 2 H2O The Pure acid CAN not be Isolated Merely by evaporating the Water, HOWEVER, Because of the Easy Oxidation of the Hypophosphorous acid to phosphoric acids (and elemental phosphorus) and its disproportionation to phosphine and phosphorous acid. The pure acid can be obtained by extraction of its aqueous solution by diethyl ether. Pure hypophosphorous acid forms white crystals that melt at 26.5 ° C. The electronic structure of hypophosphorous acid is such that it has only one hydrogen atom bound to oxygen, and thus it is a monoprotic oxyacid. It is a weak acid and forms only one series of salts, the hypophosphites. Hydrated sodium hypophosphite, NaH2PO2 × H2O, is used Reducing Industrial as an agent, as particularly for the electroless Nickel Plating of metals and nonmetals ONTO. Hypophosphorous acid from Sodium hypophosphite To a Stirred Solution of 717.8 g of a 32% HYDROCHLORIC acid Solution in a 3-necked 2 liter Flask was added 615.42 g of powdered sodium hypophosphite. The temperature of the solution rose about 2 ° C. Water was removed from the stirred reaction mixture by reduced pressure distillation at a temperature of about 55 ° C ± 7 ° C at a pressure of 44-72 mmHg until a hypophosphorous acid Concentration of about 80 wt% was Obtained. After Cooling to room temperature, Sodium chloride was Filtered That HAD Precipitated from the Reaction Mixture. The filter cake was Washed with 32 wt% Twice HYDROCHLORIC acid. The Product Contained Recovered 355.7 g of Hypophosphorous acid . The analysis showed that the product contained 0.9 wt% sodium, 3.2 wt% chloride, and 80.96 wt% hypophosphorus acid. Chloride ion was removed from hypophosphorous acid using an ion-exchange column (height 221/4 ", diameter 11/8" ). The column was packed with Rohm and Haas Resin IRA-410 in the chloride form and was Regenerated using 5% NaOH. The results from using this column at Different Concentrations H3PO2 and Cl- Shown below are. Influent Composition Composition Effluent H3PO2% Chloride % 46 3.0 49.6 0.06 46 3.0 46.7 0.09 71 5.9 52.6 0.02 Ephedrine to Methamphetamine Reduction with Hypophosphorus Acid and Iodine By Wizard X I Would Recommend a large Excess of Reducing agent for Quick Reduction. Charge Flask with 100 ml (0.1Lt) of 50% H3PO2 (0.965 mole H3PO2 per 100 ml) fit reflux condenser, add 3x33 grams (99 grams, 0.39 mole) portions of I2 while cooling in ice bath down the reflux condenser [1]. After addition of I2, gently heat so HI gas is evolving from the condenser, add 5 mls potions of H2O down the condenser till HI gas stops evolving and hence maximum amount of HI saturation kept in solution is acheived. Now add 50.4 g (0.25 mole) of ephedrine hydrochloride and boil under reflux for at least 2 hours, let cool and then made ​​basic with 20% sodium hydroxide solution (20 grams NaOH in 100 mls H2O) in ice bath to liberate the free base. Set-up glassware for steam distillation and steam distil until the distillate is almost neutral to Litmus. [2] The libertated Which seperates Methamphetamine freebase is solvent Extracted with Three, 50-75 ml ether (or Toluene) Portions and the ether / amine Washed Solution is first with 50 MLS of Distilled Water and the ether / amine Dried with Solution . anhydrous Sodium carbonate [3] After Removal of the ether (or Toluene), the Distilled Vacuum Oil was at a Vacuum of 15 mmHg at 93 ° C The yield is 80 - 82% [4].. Notes: If I2 Sticks to the Condenser Wall, Wash down with Distilled Water. Have the Distillate Receiving Flask in ice. And cool down to 4-5 degC. Anhydrous Magnesium sulphate CAN be Used. Rinse the anhydrous Magnesium sulphate with a Little ether (or Toluene) after drying the main ether / amine Solution. Ephedrine Reduction Major Reduction Reaction: C6H5- (CHOH) -CH (NHCH3) -CH3 + HI =====> C6H5- (CHI) -CH (NHCH3) -CH3 + H2O C6H5- (CHI ) -CH (NHCH3) -CH3 + HI =====> C6H5-CH2-CH (NHCH3) -CH3 + I2 Minor Reduction Reaction: C6H5- (CHI) -CH (NHCH3) -CH3 + H3PO2 + H2O == ===> C6H5-CH2-CH (NHCH3) -CH3 + H3PO3 + HI Ratio of ephedrine to HI is theoretically 1: 2, HOWEVER a 1: 3 is Used for Better Reduction and yeild. Hypophosphorus to HI Calculations H3PO2 + H2O + I2 == >> H3PO3 + 2HI Hypophosphorous 50% w / w FW = 66 g / mol Density = 1.274 g / ml... 100mls (0.1Lt) of Hypophosphorous 50% w / w contains: (1.274 / 50) / 100 = 0.637 g / ml H3PO2 = 0.00965 mol / ml H3PO2. 0.00965 mol / ml H3PO2 x 100 = 0.965 mol / 100 ml H3PO2. OR (0.637 / 66) x 1000 = 9.65 moles H3PO2 per 1000 MLS. (mol / Lt) Since WE use 100mls (0.1Lt), then 9.65 x 0.1 = 0.965 mol / 100ml H3PO2 Now since the ratio of Ephedrine:. HI is 1: 3 = (3/1), we require 0.75 moles of HI for every 0.25 moles of ephedrine hydrochloride . Since we have 0.965 mol of H3PO2 and 0.39 moles of I2 (99 / 253.8 = 0.39), then the ratio of I2: HI is 1: 2 = (2/1); so 0.39 moles of I2 reacts with the Hypophosphorous acid to . form 0.39 x 2 = 0.78 moles of HI Finally, the Excess Hypophosphorous acid, H3PO2 is 0.965-0.39 = 0.575 moles of H3PO2 is Excess The ratio for H3PO2:. I2 is 1: 1, so only 0.39 moles of H3PO2 is needed to REACT with 0.39 moles of I2 to form 0.78 moles of HI Not only do WE have enough HI;.. 0.78 moles to 0.25 moles of ephedrine hydrochloride reduce, BUT a large Excess of 0.575 moles of H3PO2 Alternatively, Charge a 1000 ml Flask with 100 ml (0.1Lt) of 50% H3PO2 (0.965 mole H3PO2 per 100 ml), 100 mls of distilled water, fit reflux condenser, add 4x49.5 grams (198 grams, 0.78 mole) portions of I2 while cooling in ice bath down the reflux condenser [1]. After addition of I2, gently heat so HI gas is evolving from the condenser, add 10 mls potions of H2O down the condenser till HI gas stops evolving and hence maximum amount of HI saturation kept in solution is acheived. Now add 100.8 g (0.5 mole) of ephedrine hydrochloride and boil under reflux for at least 2 hours, let cool and then made ​​basic with 20% sodium hydroxide solution (20 grams NaOH in 100 mls H2O) in ice bath to liberate the free base. Set -UP Glassware for Steam Distillation and Steam distil Almost until the Distillate is neutral to Litmus [2]. Since WE have 0.965 mol of H3PO2 and 0.78 moles of I2 (198 / 253.8 = 0.78), then the ratio of I2: HI is 1 : 2 = (2/1); so 0.78 moles of I2 reacts with the Hypophosphorous acid to form 0.78 x 2 = 1.56 moles of HI Finally, the excess hypophosphorus acid, H3PO2 is 0.965-0.78 = 0.185 moles of H3PO2 is excess.. The ratio for H3PO2: I2 is 1: 1, so only 0.78 moles of H3PO2 is needed to react with 0.78 moles of I2 to form 1.56 moles of HI Not only do we have enough HI; 1.56 moles to reduce 0.5 moles of ephedrine hydrochloride. , BUT an Excess of 0.185 moles of H3PO2. P-fed Reduction to Methamphetamine with Hypophosphorus Acid and Iodine By Pebble Assuming That you have Extracted P-fed from your pills, you are now READY to convert the P-fed to Methamphetamine. The structure of P-fed is so closly Related to Methamphetamine, That People have Learned to alter it's structure in Order to convert it to Methamphetamine. What one is Actually doing is Reducing a benzylic alcohol. In our Case, it Appears as OH in P-fed . So, WE strip this off completly and throw on an Additional H (Hydrogen) to the P-fed. So, by Removing the OH and H Adding a Altered THUS WE have the structure and have Created Methamphetamine. This is for Small-Scale reduction of P-fed to methamphetamine. If one wanted to make meth in the range of ounces, etc. I would not reccomend one cook in an open container. Fire or explosion are at a much higher risk when cooking anything above 10 grams using this procedure. This is why the Push / Pull apparatus is so popular. No, fumes, smell, and IT CAN reduce the risk of injury if something does go wrong. Notice I said IT CAN. There is no fool-proof method of safety when Working with Chemicals of this Nature, unless proper Lab Equipment, etc are Used; and this does not elimanate the Dangers Still, just an Accident That reduces [the probability Will happen. If one Wanted to have 5 grams as Their Finished peoduct, than 6- 8 grams of P-fed. Some get 90% yield CAN May where others only get 35% yield. This Takes time to Perfect, Will Vary WITH YOU BUT results. Take your 8 grams of P-fed and put this into a 250 ml. flask or pyrex meassuring cup. Slowing add Iodine crystals unto the p-fed is mixed well with the

النتائج (الإنجليزية) 3:

50-75毫升醚(或甲苯)部分,醚/胺解決問題,首先與50MLS的蒸餾水沖水和醚/胺干,干碳酸鈉解決辦法。[3]搬遷後的醚(或)甲苯的石油是在一個真空蒸餾真空15mmHg在93C 的收益率是80-82進行 4].

注:

如果一2堅持電容器牆、洗滌打倒 蒸餾水.
OF THE Preparation Hypophosphorus Acid Preparation of the Sodium Hypophosphite (Brit. Pat. 803,179) to the 115 g of white phosphorous is emulsified and reacted with aqueous NaOH to obtain 270 G NaH 2 PO 2. H 2 O (70 per cent). The Preparation of the aqueous sodium hypophosphite (Jap. Pat. 58185412) to theWhite phosphorus is dispersed together with slaked lime used as an assistant in an aqueous medium by stirring in an atmosphere under inert gas heating at or above the melting point of white phosphorus. The dispersion is mixed with a solution of caustic soda under heating and stirring to effect the reaction of the components. The product is separated into solid and liquid.And the mother liquor is added with a donor phosphate such as phosphoric acid. When phosphate donor is the phosphoric acid, its amount is about 0.6 mol per 1 mol dissolved of calcium, and the pH of the system is usually maintained to about 8-11. The reaction is carried out at about 50-100°C, and the reaction for product is aged about 30 min.The Ca (II) dissolved in the mother precipitated liquid is in the form of apatite calcium, and the high-purity of sodium hypophosphite aqueous solution can be recovered by this process. The Hypophosphorous acid) The purification Free the hypophosphorous acid, H 3 PO 2, is prepared by acidifying aqueous solutions of hypophosphite ions, H 2 PO 2-. For example.The remaining solution when phosphine is prepared from the reaction of white phosphorus and a base contains the H 2 PO 2-ion. If barium hydroxide, Ba (OH) 2, is used as the base and the solution is acidified with sulfuric acid, barium sulfate, precipitates and an aqueous solution of hypophosphorous acid results. The Ba the 2 2 H 2 PO 2-2 H 3 O SO 42-=> BaSO 4 2 H 3 PO 2 2 H 2 O))The pure acid cannot be isolated merely by evaporating the water, however, because of the easy oxidation of the hypophosphorous phosphoric acid to acids (and elemental phosphorus) and its disproportionation to phosphine phosphorous and acid. The pure acid can be obtained by extraction of its aqueous solution by diethyl ether. Pure hypophosphorous acid forms white crystals that melt at 26.5°C.The electronic structure of hypophosphorous acid is such that it has only one hydrogen atom bound to oxygen, and thus it is a monoprotic oxyacid. It is a weak acid and forms only one series of salts, the hypophosphites. Hydrated sodium hypophosphite, NaH 2 PO 2 × H 2 O, is used as an industrial reducing agent, particularly for the electroless plating of nickel onto metals and nonmetals.))