Introduction
There is simple piperine extraction method from black paper. Piperine can be used as several step precursor for MDMA synthesis.Reagents:
- Ground black pepper 300 g;
- Ethanol 616 ml (88%);
- Potassium hydroxide (KOH) 24 g;
- Distilled water ~1 L;
- Soxhlet extractor 500 ml;
- Round or flat bottom flask;
- Reflux condenser;
- Filter paper sleeves [special cellulose thimbles can be used instead of filter paper sleeve];
- Paper filter;
- Desiccator with alkali or vacuum;
- Freezer;
- Boiling chips;
- Retort stand and clamp for securing apparatus;
- Beakers (1 L; 500 ml; 250 ml x2, 100 ml x 2);
- Heating plate;
- Laboratory scale (0.1-200 g is suitable);
- Plastic spoon;
- pH indicator paper;
- Glass rod and spatula;
Procedures
Stage 1. Piperine Extraction
1. Ground black pepper 300 g is 5 extraction batches of 60 g each.
2. A filter paper sleeve is placed in the Soxhlet extractor.
3. Ground black pepper is poured into the sleeve.
4. Ethanol 400 ml (88%) is poured into the flask with boiling chips and the extraction device is assembled.
5. Alcohol is brought to the boiling point and the extraction process is begun.
6. The alcohol condensation cycle is repeated until colorless ethanol drained from the sleeve.
7. When ethanol is become colorless, the next portion of ground pepper (60 g) is placed in the sleeve.
Stage 2. Isolation of Piperine
9. Potassium hydroxide is dissolved in ethanol.
10. The resulting black pepper extract is filtered through a paper filter directly into the prepared KOH ethanol solution.
11. The resulting solution is heated to 60-70℃.
12. Distilled water (about 1 L) is poured into the heated solution in portions until the formation of a yellow piperine precipitate is stopped.
13. The resulting suspension is cooled in the freezer for 24h.
14. The precipitate is filtered through a paper filter.
15. The filtered piperine precipitate is dried in a desiccator over alkali or under a fan heater to a constant weight.
16. The precipitate should have a slight pepper smell and a melting point 127-128°C.
17. The extraction piperine yield is 17 g.
1. Ground black pepper 300 g is 5 extraction batches of 60 g each.
2. A filter paper sleeve is placed in the Soxhlet extractor.
3. Ground black pepper is poured into the sleeve.
4. Ethanol 400 ml (88%) is poured into the flask with boiling chips and the extraction device is assembled.
5. Alcohol is brought to the boiling point and the extraction process is begun.
6. The alcohol condensation cycle is repeated until colorless ethanol drained from the sleeve.
7. When ethanol is become colorless, the next portion of ground pepper (60 g) is placed in the sleeve.
Note: Alcohol in the flask shouldn't be replaced during the entire extraction process.
8. Thus, extraction is continued until the entire amount of ground pepper is finished.Stage 2. Isolation of Piperine
9. Potassium hydroxide is dissolved in ethanol.
10. The resulting black pepper extract is filtered through a paper filter directly into the prepared KOH ethanol solution.
11. The resulting solution is heated to 60-70℃.
12. Distilled water (about 1 L) is poured into the heated solution in portions until the formation of a yellow piperine precipitate is stopped.
13. The resulting suspension is cooled in the freezer for 24h.
14. The precipitate is filtered through a paper filter.
15. The filtered piperine precipitate is dried in a desiccator over alkali or under a fan heater to a constant weight.
16. The precipitate should have a slight pepper smell and a melting point 127-128°C.
17. The extraction piperine yield is 17 g.
