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Phenylacetone (P2P): 100 mL (~101 g, 0.753 mol).
Ammonia: 150–200 mL of 25% aqueous solution (~37.5–50 g NH3, 2.2–2.9 mol). Sufficient excess to form the imine.
NaBH4: 10–15 g (0.26–0.40 mol). For 0.753 mol of P2P, ~0.19–0.38 mol of NaBH4 is required, so the range is suitable.
Acetic acid (CH3COOH): 5–10 mL (to adjust pH to 4–6).
Sodium bicarbonate (NaHCO3): 20–50 g or 100–200 mL of 10% solution (~10–20 g NaHCO3). Sufficient for neutralization.
Methanol: 200–250 mL. Suitable as a reaction solvent.
Dichloromethane (optional): 100–150 mL (for free base extraction).
Water: 200–300 mL (for dilution and washing).
HCl: 10–20 mL of a 37% solution (for hydrochloride formation).
Acetone: 50–100 mL (for crystallization and washing).
Required materials: Indicator paper, filter paper, optional TLC plates.
Steps for preparing the mixture:
In a 500 mL flask, pour 100 mL of P2P and 200 mL of methanol.
Add 150–200 mL of 25% ammonia solution.
Slowly add 5–10 mL of acetic acid, monitoring the pH (4–6) with pH paper.
Stir at room temperature (~20–25°C) for 1 hour (imine formation).
Reduction:
In a fume hood, slowly add 10–15 g of NaBH4 in portions over 30–60 minutes, maintaining the temperature <40°C (e.g., water bath).
Stir for 4–6 hours at room temperature.
Neutralization:
Slowly add 100–200 mL of 10% NaHCO3 solution or 20–50 g of powder until the pH reaches ~7. Beware of foaming (CO2) and hydrogen (H2).
Filter the mixture through a filter paper to remove precipitates (e.g., borates).
Purification:
(Optional) Dilute the mixture with water (~200 mL) and extract with dichloromethane (3 x 50 mL). Dry the organic layer with MgSO4 and evaporate the solvent.
Evaporate the methanol and water (~40–60°C) using a rotary evaporator or with gentle heating to obtain an oil (amphetamine free base).
Dissolve the oil in acetone (50 mL), add 37% HCl (10–20 mL) to a pH of ~5–6 until amphetamine hydrochloride precipitates.
Filter the powder and rinse with cold acetone (~10–20 mL).
Sorry for the language but I use a translator
The previous one was deleted by the Polish language.
Please tell me if this is possible and if anything will come of it.
Phenylacetone (P2P): 100 mL (~101 g, 0.753 mol).
Ammonia: 150–200 mL of 25% aqueous solution (~37.5–50 g NH3, 2.2–2.9 mol). Sufficient excess to form the imine.
NaBH4: 10–15 g (0.26–0.40 mol). For 0.753 mol of P2P, ~0.19–0.38 mol of NaBH4 is required, so the range is suitable.
Acetic acid (CH3COOH): 5–10 mL (to adjust pH to 4–6).
Sodium bicarbonate (NaHCO3): 20–50 g or 100–200 mL of 10% solution (~10–20 g NaHCO3). Sufficient for neutralization.
Methanol: 200–250 mL. Suitable as a reaction solvent.
Dichloromethane (optional): 100–150 mL (for free base extraction).
Water: 200–300 mL (for dilution and washing).
HCl: 10–20 mL of a 37% solution (for hydrochloride formation).
Acetone: 50–100 mL (for crystallization and washing).
Required materials: Indicator paper, filter paper, optional TLC plates.
Steps for preparing the mixture:
In a 500 mL flask, pour 100 mL of P2P and 200 mL of methanol.
Add 150–200 mL of 25% ammonia solution.
Slowly add 5–10 mL of acetic acid, monitoring the pH (4–6) with pH paper.
Stir at room temperature (~20–25°C) for 1 hour (imine formation).
Reduction:
In a fume hood, slowly add 10–15 g of NaBH4 in portions over 30–60 minutes, maintaining the temperature <40°C (e.g., water bath).
Stir for 4–6 hours at room temperature.
Neutralization:
Slowly add 100–200 mL of 10% NaHCO3 solution or 20–50 g of powder until the pH reaches ~7. Beware of foaming (CO2) and hydrogen (H2).
Filter the mixture through a filter paper to remove precipitates (e.g., borates).
Purification:
(Optional) Dilute the mixture with water (~200 mL) and extract with dichloromethane (3 x 50 mL). Dry the organic layer with MgSO4 and evaporate the solvent.
Evaporate the methanol and water (~40–60°C) using a rotary evaporator or with gentle heating to obtain an oil (amphetamine free base).
Dissolve the oil in acetone (50 mL), add 37% HCl (10–20 mL) to a pH of ~5–6 until amphetamine hydrochloride precipitates.
Filter the powder and rinse with cold acetone (~10–20 mL).