WillD
Expert
- Joined
- Jul 19, 2021
- Messages
- 729
- Reaction score
- 1,037
- Points
- 93
Reagents:
Synthesis:
- Lithium aluminum hydride (LAH; cas 16853-85-3) 12 g;
- 1,4-Dioxane 300 ml;
- 1-Phenyl-2-nitropropene (P2NP; cas 705-60-2) 10 g;
- Sodium hydroxide (25% NaOH) aq. solution;
- Acetone ~50 ml;
- Sulfuric acid ~10 ml;
- Two-naked round bottom flask 1 L;
- Magnetic or top stirrer;
- Beakers 200 ml x3;
- Drip funnel;
- pH Indicator paper;
- Laboratory scale (0.1-200 g is suitable);
- Measuring cylinder 100 mL;
- Glass rod and spatula;
- Rotovap machine (optional);
- Water bath with ice;
- Funnel;
- Filter paper;
- Buchner flask and funnel;
- Freezer;
Synthesis:
1. Lithium aluminum hydride (LAH) 12 g is weighted and put into a 1 L two-naked round bottom flask.
2. 1,4-Dioxane 200 ml is added into the flask.
3. The flask is places onto a magnetic stirrer and clamped on a retort stand, stirring bar is placed into the flask.
4. 1-Phenyl-2-nitropropene (P2NP) 10 g and 1,4-dioxane 100 ml are mixed in a 200 mL beaker. The mixture is stirred at room temperature until 1-Phenyl-2-nitropropene (P2NP) is dissolved.
5. A drip funnel is installed onto a reaction flask neck. The P2NP solution from step 4 is poured into the drip funnel.
6. A drip funnel tap is opened and solution from step 4 is poured dropwise into the reaction mixture.
7. The reaction mixture is stirred at room temperature for 30 min after complete P2NP solution addition.
8. Reflux condenser is installed onto the flask and the reaction mixture is refluxed for 1 h.
9. Then, the reaction flask is cooled in an ice water bath.
10. LAH is decomposed by the slow sodium hydroxide (25% NaOH aq. solution) addition.
11. The resulting white suspension is filtered from solids. Organic layer is separated with help of separatory funnel.
12. Organic layer is evaporated under reduced pressure. Amphetamine free base yellow oil is obtained.
13. The amphetamine free base oil is dissolved in x3 acetone volume.
14. Sulfuric (or orthophosphoric) acid is added dropwise with a constant stirring to reach pH 6.
15. The mixture is put into a freezer for 12 hours.
16. Next, the mixture is filtered on a Buchner flask and funnel. Amphetamine sulphate salt is air dried or dried in a vacuum desiccator.
2. 1,4-Dioxane 200 ml is added into the flask.
3. The flask is places onto a magnetic stirrer and clamped on a retort stand, stirring bar is placed into the flask.
4. 1-Phenyl-2-nitropropene (P2NP) 10 g and 1,4-dioxane 100 ml are mixed in a 200 mL beaker. The mixture is stirred at room temperature until 1-Phenyl-2-nitropropene (P2NP) is dissolved.
5. A drip funnel is installed onto a reaction flask neck. The P2NP solution from step 4 is poured into the drip funnel.
6. A drip funnel tap is opened and solution from step 4 is poured dropwise into the reaction mixture.
7. The reaction mixture is stirred at room temperature for 30 min after complete P2NP solution addition.
8. Reflux condenser is installed onto the flask and the reaction mixture is refluxed for 1 h.
9. Then, the reaction flask is cooled in an ice water bath.
10. LAH is decomposed by the slow sodium hydroxide (25% NaOH aq. solution) addition.
11. The resulting white suspension is filtered from solids. Organic layer is separated with help of separatory funnel.
12. Organic layer is evaporated under reduced pressure. Amphetamine free base yellow oil is obtained.
13. The amphetamine free base oil is dissolved in x3 acetone volume.
14. Sulfuric (or orthophosphoric) acid is added dropwise with a constant stirring to reach pH 6.
15. The mixture is put into a freezer for 12 hours.
16. Next, the mixture is filtered on a Buchner flask and funnel. Amphetamine sulphate salt is air dried or dried in a vacuum desiccator.
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