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- Jan 7, 2024
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Step-by-Step Recipe
Initial Setup
- Prepare the Solvent Mixture:
- Measure 25 mL of Isopropyl Alcohol (IPA) (5 times the weight of P2NP).
- Add 5 mL of distilled water (20% of the total volume of IPA).
- Mark Liquid Level:
- Mark the liquid level on the side of the reaction vessel for future reference.
- Start Stirring:
- Turn on the stirring apparatus to medium speed.
Reduction Reaction
- Add Sodium Borohydride:
- Weigh 6.87 g of granular sodium borohydride (6 molar equivalents based on 5 g of P2NP).
- Add P2NP:
- Gradually add 5 g of P2NP in small portions to control frothing and temperature.
- Monitor the Reaction:
- Continue stirring until the yellow solution decolorizes, indicating the reduction is progressing.
- Top Up with IPA:
- If necessary, add additional IPA to maintain the initial liquid level.
- Add More Sodium Borohydride:
- Add an additional 2.29 g of sodium borohydride (2 molar equivalents).
Addition of Copper Chloride Dihydrate
- Prepare Copper Chloride Solution:
- Dissolve 0.93 g of CuCl2·2H2O (18% molar equivalent) in a small amount of distilled water.
- Add Copper Chloride Solution:
- Add the solution in one go with vigorous overhead stirring.
- Allow Reaction to Complete:
- Continue stirring for 40 minutes to allow the formation of the copper nanoparticle catalyst and reduction of the nitro group to the amine group.
Quenching and Distillation
- Quench the Reaction:
- Slowly add a dilute acetic acid solution until the pH reaches 3.
- Distillation Setup:
- Set up a short path distillation apparatus and distill off everything up to 96°C to remove the IPA.
Extraction of Amine
- Adjust pH with NaOH:
- Add 25% NaOH solution until the pH reaches 12.
- Steam Distillation:
- Set up for steam distillation using a vertical steam head connected to a wallpaper steamer filled with deionized water.
- Distill directly into a 2L separatory funnel connected to a condenser.
- If the funnel becomes more than 75% full, drain off some water.
- Collect Amine:
- Collect the clear amine oil that floats on top of the water.
Salting Out and Drying
- Salt Out the Aqueous Layer:
- Return the water to the separatory funnel and add enough NaCl to saturate it (around 350 g/L).
- Shake well and allow to settle for a few hours.
- Separate the aqueous and organic layers again.
- Combine Organic Extracts:
- Combine the organic amine extracts and dry over molecular sieves (3A) for 6 hours.
- Filter:
- Filter out the molecular sieves to obtain the dried amine oil.
Final Reaction to Form Amphetamine Sulfate
- Prepare Amine-IPA Mixture:
- Mix the amine oil with an equal volume of dry IPA.
- Calculate and Add Sulfuric Acid:
- Calculate the amount of H2SO4 needed based on your yield (e.g., 0.06 moles of H2SO4, which equals 5.88 g).
- Dilute the sulfuric acid in twice its volume of dry IPA and add dropwise to the amine-IPA mixture until pH 7.
- Crystallization:
- Filter the resulting amphetamine sulfate using a Buchner funnel and vacuum.
- Test the filtrate for pH and adjust if necessary by adding more acid dropwise until pH 7.
- Final Filtration:
- Leave the crystal slurry in a cold fridge overnight, then filter again on the Buchner funnel.
- Dry the Product:
- Allow the amphetamine sulfate to dry completely, yielding a white amorphous solid.