Amphetamine Synthesis of Amphetamine from P2NP with NaBH4/CuCl2 (for 1 kg)

[ireshop]

Reaction scheme:

Laboratory equipment and materials :

• 50 L reactor with reflux condenser, stirrer on top and configured with heater.
• Trickling funnel.
• Conventional funnel.
• Laboratory thermometer (measurement up to 150 °С).
• Several 10 and 20 L buckets.
• 1 L measuring cylinder.
• Vacuum pump.
• Laboratory weighing scale (suitable for 1-2000 g).
• Cold water bath source for reflux condenser.
• Nutsche filter.
• pH measuring papers.
• 2 x 5 L beakers.
• Freezer.
• Pyrex dishes for crystallisation.

Reagents:

• Isopropyl alcohol (IPA) 20 L.
• Distilled water 6.2 L.
• Sodium borohydride (NaBH4) 1739 g.
• P2NP (phenyl-2-propanone) 1000 g.
• Copper (II) chloride (CuCl2) 105 g.
• Sodium hydroxide (NaOH) 25% aqueous solution 8 L.
• Anhydrous acetone 2.5 L.
• Sulphuric acid (or ortho-phosphoric acid).

Synthesis:

1. A mixture of IPA and H2O in a 2:1 ratio (18 litres) is added to a 50 L reactor.
2. Solid NaBH4 (1739 g) is added at once and the stirrer is switched on.
3. Pure P2NP (1000 g) is added in several small doses to keep the temperature of the mixture below 60 °С.
4. A solution of CuCl2 (105 g) in water (200 ml) is added slowly dropwise to keep the temperature of the mixture below 80 °С.
5. Subsequently, the reaction is maintained at 80 °C for 30 minutes with the aid of external heating.
6. An aqueous NaOH solution (8 litres at 25 %) is added to the reaction mixture and the layers are separated.
7. The aqueous phase is extracted with 8 litres of IPA. The free amphetamine base is dissolved in IPA and the density of the IPA layer changes, thus separating it from the aqueous layer.
8. The IPA from the extract of step 7 is evaporated under vacuum to an amphetamine-free base oil and combined with the free base from step 6.
9. The amphetamine-free base oil is dissolved in 2 L of anhydrous acetone.
10. Sulphuric acid (or ortho-phosphoric acid) is added dropwise until a pH of 6 is reached (with constant stirring).
11. The mixture is then placed in a freezer for 12 hours.
12. After the crystallisation procedure in the freezer, the amphetamine salt suspension is filtered through a Nutsche filter and washed with cold anhydrous acetone until a white colour is obtained. The washing procedure can be crystallised as described in steps 11-12 (the quality of the amphetamine salt from this solution will be lower). The yield of the reaction is 60-70 %.