Synthesis of Amphetamine from P2NP via SnCl2 and Zn

TucoSalamanca.

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How can I tell if it's amphetamines?
 

GDC

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TucoSalamanca.

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4.039 g of sodium carbonate to replace the 25 g of sodium hydroxide. You can dissolve this amount of sodium carbonate in 50 ml of water to achieve a similar concentration as the original NaOH solution.

32.30 g of sodium carbonate to replace the 100 g of sodium hydroxide. You can dissolve this amount of sodium carbonate in 100 ml of water to achieve a similar concentration as the original NaOH solution.
GDCIs 32,30 g sodium carbonate in 100 ml water correct?
 
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TucoSalamanca.

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4.039 g of sodium carbonate to replace the 25 g of sodium hydroxide. You can dissolve this amount of sodium carbonate in 50 ml of water to achieve a similar concentration as the original NaOH solution.

32.30 g of sodium carbonate to replace the 100 g of sodium hydroxide. You can dissolve this amount of sodium carbonate in 100 ml of water to achieve a similar concentration as the original NaOH solution.

So:
7,5 g of P2NP in ~25 ml of anhydrous acetone
~25ml acetone and 21 g of tin(II) chloride dihydrate
75 ml of cold water and 2 ml 36% hydrochloric acid
Na2CO3 (32,30g per 100ml of water)
3 x 25 ml portions of ethyl acetate
30 ml glacial acetic acid
5 g of zinc dust.
4,039 g Na2CO3 in 50 ml water
25 ml dichloromethane
3x 10 ml DCM.
anhydrous magnesium sulfate ~1/20 of the final solution
25 ml of anhydrous acetone
GDCAm I seeing it wrong? You wrote 4039 grams.
 

TucoSalamanca.

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4.039 g of sodium carbonate to replace the 25 g of sodium hydroxide. You can dissolve this amount of sodium carbonate in 50 ml of water to achieve a similar concentration as the original NaOH solution.

32.30 g of sodium carbonate to replace the 100 g of sodium hydroxide. You can dissolve this amount of sodium carbonate in 100 ml of water to achieve a similar concentration as the original NaOH solution.

So:
7,5 g of P2NP in ~25 ml of anhydrous acetone
~25ml acetone and 21 g of tin(II) chloride dihydrate
75 ml of cold water and 2 ml 36% hydrochloric acid
Na2CO3 (32,30g per 100ml of water)
3 x 25 ml portions of ethyl acetate
30 ml glacial acetic acid
5 g of zinc dust.
4,039 g Na2CO3 in 50 ml water
25 ml dichloromethane
3x 10 ml DCM.
anhydrous magnesium sulfate ~1/20 of the final solution
25 ml of anhydrous acetone
GDCDoes it say 4 grams?
 
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GDC

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I think the synthesis failed because I poured the hcl and cold water too fast.
TucoSalamanca.This Reaction take more time as the Thread opener wrote....
Steps and timeframes:
  1. Reaction setup (15-30 minutes): Dissolve the oxime in GAA in a round-bottom flask.
  2. Reduction (4-8 hours):
    1. Add zinc powder to the reaction mixture,
    2. heat it to reflux, and maintain the temperature until the reaction is complete.
  3. Neutralization (10-20 minutes):
    1. Slowly add a solution of NaOH to the mixture to neutralize the excess GAA, bringing the pH to >10.
  4. Filtration (10-20 minutes):
    1. Filter the mixture through a Celite or diatomaceous earth pad to remove any insoluble zinc salts and other impurities.
  5. Separation (5-10 minutes):
    1. Partition the filtrate between an organic solvent, such as ethyl acetate, and water. Separate the organic layer from the aqueous layer.
  6. Extraction (15-30 minutes):
    1. Extract the aqueous layer with additional portions of ethyl acetate (or another suitable organic solvent) to ensure complete extraction of the product.
  7. Drying (10-20 minutes):
    1. Combine the organic layers and dry them over a drying agent like magnesium sulfate (MgSO4) or sodium sulfate (Na2SO4).
  8. Filtering and evaporation (20-40 minutes):
    1. Filter the dried organic solution to remove the drying agent, and then evaporate the solvent under reduced pressure to yield the crude product.
  9. Purification (1-3 hours):
    1. Purify the crude product using techniques like recrystallization, chromatography, or distillation, as needed.
 

TucoSalamanca.

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This Reaction take more time as the Thread opener wrote....
Steps and timeframes:
  1. Reaction setup (15-30 minutes): Dissolve the oxime in GAA in a round-bottom flask.
  2. Reduction (4-8 hours):
    1. Add zinc powder to the reaction mixture,
    2. heat it to reflux, and maintain the temperature until the reaction is complete.
  3. Neutralization (10-20 minutes):
    1. Slowly add a solution of NaOH to the mixture to neutralize the excess GAA, bringing the pH to >10.
  4. Filtration (10-20 minutes):
    1. Filter the mixture through a Celite or diatomaceous earth pad to remove any insoluble zinc salts and other impurities.
  5. Separation (5-10 minutes):
    1. Partition the filtrate between an organic solvent, such as ethyl acetate, and water. Separate the organic layer from the aqueous layer.
  6. Extraction (15-30 minutes):
    1. Extract the aqueous layer with additional portions of ethyl acetate (or another suitable organic solvent) to ensure complete extraction of the product.
  7. Drying (10-20 minutes):
    1. Combine the organic layers and dry them over a drying agent like magnesium sulfate (MgSO4) or sodium sulfate (Na2SO4).
  8. Filtering and evaporation (20-40 minutes):
    1. Filter the dried organic solution to remove the drying agent, and then evaporate the solvent under reduced pressure to yield the crude product.
  9. Purification (1-3 hours):
    1. Purify the crude product using techniques like recrystallization, chromatography, or distillation, as needed.
GDCI will use sodium hydroxide for the next synthesis alkali and I will add hcl water slowly, I added it too fast.
 

GDC

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I will use sodium hydroxide for the next synthesis alkali and I will add hcl water slowly, I added it too fast.
TucoSalamanca.He add the Oxime to the HCl / water solution :)
The rate at which 1-phenylpropan-2-one oxime can be added to an HCl solution can depend on various factors, including the concentration of the HCl solution, the temperature of the reaction mixture, and the specific experimental setup. In general, the addition should be done slowly and carefully, while monitoring the reaction to ensure it proceeds safely and as expected.
 
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GDC

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the translation is very inaccurate, I apologise for the misspelling
TucoSalamanca.The thread-opener added the 1-phenylpropan-2-one oxime (The product of P2NP + SnCL2 * 2H2O) to the solution of HCl x Water. But yes i think we have to do it slow.
 

mithyl2

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The thread-opener added the 1-phenylpropan-2-one oxime (The product of P2NP + SnCL2 * 2H2O) to the solution of HCl x Water. But yes i think we have to do it slow.
GDCtry reagent tests such as a marquis
 

hacke8

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This Reaction take more time as the Thread opener wrote....
Steps and timeframes:
  1. Reaction setup (15-30 minutes): Dissolve the oxime in GAA in a round-bottom flask.
  2. Reduction (4-8 hours):
    1. Add zinc powder to the reaction mixture,
    2. heat it to reflux, and maintain the temperature until the reaction is complete.
  3. Neutralization (10-20 minutes):
    1. Slowly add a solution of NaOH to the mixture to neutralize the excess GAA, bringing the pH to >10.
  4. Filtration (10-20 minutes):
    1. Filter the mixture through a Celite or diatomaceous earth pad to remove any insoluble zinc salts and other impurities.
  5. Separation (5-10 minutes):
    1. Partition the filtrate between an organic solvent, such as ethyl acetate, and water. Separate the organic layer from the aqueous layer.
  6. Extraction (15-30 minutes):
    1. Extract the aqueous layer with additional portions of ethyl acetate (or another suitable organic solvent) to ensure complete extraction of the product.
  7. Drying (10-20 minutes):
    1. Combine the organic layers and dry them over a drying agent like magnesium sulfate (MgSO4) or sodium sulfate (Na2SO4).
  8. Filtering and evaporation (20-40 minutes):
    1. Filter the dried organic solution to remove the drying agent, and then evaporate the solvent under reduced pressure to yield the crude product.
  9. Purification (1-3 hours):
    1. Purify the crude product using techniques like recrystallization, chromatography, or distillation, as needed.
GDCHello, sir, ethyl acetate is used in it. Can petroleum ether or xylene be replaced in the fifth part? Can I use a solvent to complete all the extraction?
 

GDC

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Hello, sir, ethyl acetate is used in it. Can petroleum ether or xylene be replaced in the fifth part? Can I use a solvent to complete all the extraction?
hacke8Sorry, but i'm not the thread creator.
maybe @G.Patton know that.
"The first was ethyl acetate, the second was dichloromethane, and the third was DCM."
DCM is DiChlorMethane :)
And i think ethyl acetate isn't a problem or?
And yes you can replace DCM with ether
 

GDC

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you have to check density
 

hacke8

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Sorry, but i'm not the thread creator.
maybe @G.Patton know that.
"The first was ethyl acetate, the second was dichloromethane, and the third was DCM."
DCM is DiChlorMethane :)
And i think ethyl acetate isn't a problem or?
And yes you can replace DCM with ether
GDCThank you for your reply. I know that DCM is dichloromethane. I don't know whether ethyl acetate is a reactant or an extractant. If it is a reactant, it may not be replaceable. If the extraction agent is replaced with petroleum ether or xylene, will it affect the subsequent reaction?
 

hacke8

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Thank you very much for your selfless sharing. I have a few questions to ask you. 1: Can 37% hydrochloric acid be used directly when adding water and hydrochloric acid? 2: What is the PH value after adding hydrochloric acid? 3: Three solvents were used to extract during the experiment. The first was ethyl acetate, the second was dichloromethane, and the third was DCM. I would like to ask if these three extractions can be replaced by petroleum ether or xylene, or which solvent is irreplaceable?
 
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