- Joined
- May 7, 2023
- Messages
- 130
- Reaction score
- 12
- Points
- 18
How can I tell if it's amphetamines?
- Joined
- Apr 30, 2022
- Messages
- 41
- Reaction score
- 8
- Points
- 8
How can I tell if it's amphetamines?
↑View previous replies…
GDCIs 32,30 g sodium carbonate in 100 ml water correct?
GDCAm I seeing it wrong? You wrote 4039 grams.
GDCDoes it say 4 grams?
TucoSalamanca.This Reaction take more time as the Thread opener wrote....
Steps and timeframes:
GDCI 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.
GDCthe 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.
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?
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
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?
- Joined
- May 7, 2023
- Messages
- 130
- Reaction score
- 12
- Points
- 18
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.
- Joined
- Apr 30, 2022
- Messages
- 41
- Reaction score
- 8
- Points
- 8
- Joined
- May 7, 2023
- Messages
- 130
- Reaction score
- 12
- Points
- 18
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
- Joined
- May 7, 2023
- Messages
- 130
- Reaction score
- 12
- Points
- 18
- Joined
- May 7, 2023
- Messages
- 130
- Reaction score
- 12
- Points
- 18
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
- Joined
- Apr 30, 2022
- Messages
- 41
- Reaction score
- 8
- Points
- 8
- Joined
- May 7, 2023
- Messages
- 130
- Reaction score
- 12
- Points
- 18
- Joined
- Apr 30, 2022
- Messages
- 41
- Reaction score
- 8
- Points
- 8
I think the synthesis failed because I poured the hcl and cold water too fast.
Steps and timeframes:
- Reaction setup (15-30 minutes): Dissolve the oxime in GAA in a round-bottom flask.
- Reduction (4-8 hours):
- Add zinc powder to the reaction mixture,
- heat it to reflux, and maintain the temperature until the reaction is complete.
- Neutralization (10-20 minutes):
- Slowly add a solution of NaOH to the mixture to neutralize the excess GAA, bringing the pH to >10.
- Filtration (10-20 minutes):
- Filter the mixture through a Celite or diatomaceous earth pad to remove any insoluble zinc salts and other impurities.
- Separation (5-10 minutes):
- Partition the filtrate between an organic solvent, such as ethyl acetate, and water. Separate the organic layer from the aqueous layer.
- Extraction (15-30 minutes):
- Extract the aqueous layer with additional portions of ethyl acetate (or another suitable organic solvent) to ensure complete extraction of the product.
- Drying (10-20 minutes):
- Combine the organic layers and dry them over a drying agent like magnesium sulfate (MgSO4) or sodium sulfate (Na2SO4).
- Filtering and evaporation (20-40 minutes):
- Filter the dried organic solution to remove the drying agent, and then evaporate the solvent under reduced pressure to yield the crude product.
- Purification (1-3 hours):
- Purify the crude product using techniques like recrystallization, chromatography, or distillation, as needed.
- Joined
- May 7, 2023
- Messages
- 130
- Reaction score
- 12
- Points
- 18
This Reaction take more time as the Thread opener wrote....
Steps and timeframes:
- Reaction setup (15-30 minutes): Dissolve the oxime in GAA in a round-bottom flask.
- Reduction (4-8 hours):
- Add zinc powder to the reaction mixture,
- heat it to reflux, and maintain the temperature until the reaction is complete.
- Neutralization (10-20 minutes):
- Slowly add a solution of NaOH to the mixture to neutralize the excess GAA, bringing the pH to >10.
- Filtration (10-20 minutes):
- Filter the mixture through a Celite or diatomaceous earth pad to remove any insoluble zinc salts and other impurities.
- Separation (5-10 minutes):
- Partition the filtrate between an organic solvent, such as ethyl acetate, and water. Separate the organic layer from the aqueous layer.
- Extraction (15-30 minutes):
- Extract the aqueous layer with additional portions of ethyl acetate (or another suitable organic solvent) to ensure complete extraction of the product.
- Drying (10-20 minutes):
- Combine the organic layers and dry them over a drying agent like magnesium sulfate (MgSO4) or sodium sulfate (Na2SO4).
- Filtering and evaporation (20-40 minutes):
- Filter the dried organic solution to remove the drying agent, and then evaporate the solvent under reduced pressure to yield the crude product.
- Purification (1-3 hours):
- Purify the crude product using techniques like recrystallization, chromatography, or distillation, as needed.
- Joined
- Apr 30, 2022
- Messages
- 41
- Reaction score
- 8
- Points
- 8
I will use sodium hydroxide for the next synthesis alkali and I will add hcl water slowly, I added it too fast.
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.
Last edited:
- Joined
- May 7, 2023
- Messages
- 130
- Reaction score
- 12
- Points
- 18
He add the Oxime to the HCl / water solution
- Joined
- Apr 30, 2022
- Messages
- 41
- Reaction score
- 8
- Points
- 8
the translation is very inaccurate, I apologise for the misspelling
- Joined
- Feb 26, 2024
- Messages
- 38
- Reaction score
- 4
- Points
- 8
This Reaction take more time as the Thread opener wrote....
Steps and timeframes:
- Reaction setup (15-30 minutes): Dissolve the oxime in GAA in a round-bottom flask.
- Reduction (4-8 hours):
- Add zinc powder to the reaction mixture,
- heat it to reflux, and maintain the temperature until the reaction is complete.
- Neutralization (10-20 minutes):
- Slowly add a solution of NaOH to the mixture to neutralize the excess GAA, bringing the pH to >10.
- Filtration (10-20 minutes):
- Filter the mixture through a Celite or diatomaceous earth pad to remove any insoluble zinc salts and other impurities.
- Separation (5-10 minutes):
- Partition the filtrate between an organic solvent, such as ethyl acetate, and water. Separate the organic layer from the aqueous layer.
- Extraction (15-30 minutes):
- Extract the aqueous layer with additional portions of ethyl acetate (or another suitable organic solvent) to ensure complete extraction of the product.
- Drying (10-20 minutes):
- Combine the organic layers and dry them over a drying agent like magnesium sulfate (MgSO4) or sodium sulfate (Na2SO4).
- Filtering and evaporation (20-40 minutes):
- Filter the dried organic solution to remove the drying agent, and then evaporate the solvent under reduced pressure to yield the crude product.
- Purification (1-3 hours):
- Purify the crude product using techniques like recrystallization, chromatography, or distillation, as needed.
- Joined
- Apr 30, 2022
- Messages
- 41
- Reaction score
- 8
- Points
- 8
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?
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
- Joined
- Feb 26, 2024
- Messages
- 38
- Reaction score
- 4
- Points
- 8
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