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- Joined
- Jan 14, 2024
- Messages
- 85
- Reaction score
- 48
- Points
- 18
Reaction scheme:
Laboratory equipment and materials :
Reagents:
Synthesis:
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:
- A mixture of IPA and H2O in a 2:1 ratio (18 litres) is added to a 50 L reactor.
- Solid NaBH4 (1739 g) is added at once and the stirrer is switched on.
- Pure P2NP (1000 g) is added in several small doses to keep the temperature of the mixture below 60 °С.
- A solution of CuCl2 (105 g) in water (200 ml) is added slowly dropwise to keep the temperature of the mixture below 80 °С.
- Subsequently, the reaction is maintained at 80 °C for 30 minutes with the aid of external heating.
- An aqueous NaOH solution (8 litres at 25 %) is added to the reaction mixture and the layers are separated.
- 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.
- 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.
- The amphetamine-free base oil is dissolved in 2 L of anhydrous acetone.
- Sulphuric acid (or ortho-phosphoric acid) is added dropwise until a pH of 6 is reached (with constant stirring).
- The mixture is then placed in a freezer for 12 hours.
- 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 %.