Introduction
The clandestine manufacture of MDMA is most commonly performed via a reductive amination of 3,4-methylenedioxyphenyl-2-propanone (MDP2P). Most synthetic routes leading to this precursor begin with materials that already contain a pre-installed methylenedioxyphenyl moiety such as safrole, isosafrole and piperonal.
The precursor compound piperonal could theoretically be synthesised in a clandestine setting by the oxidation of piperine, the major alkaloid present in black pepper. Piperonal could also be obtained via an oxidation reaction of piperic acid, which can be readily produced by the hydrolysis of piperine. There are multiple previous syntheses of piperonal from piperine and piperic acid, many located online on clandestine internet forums. Piperonal could be successfully synthesised from both piperine and from the commercially available flavorant vanillin.
The precursor compound piperonal could theoretically be synthesised in a clandestine setting by the oxidation of piperine, the major alkaloid present in black pepper. Piperonal could also be obtained via an oxidation reaction of piperic acid, which can be readily produced by the hydrolysis of piperine. There are multiple previous syntheses of piperonal from piperine and piperic acid, many located online on clandestine internet forums. Piperonal could be successfully synthesised from both piperine and from the commercially available flavorant vanillin.
This work examines the chemical synthesis of piperic acid from piperine prepared via alkaline hydrolysis. This step is important step in MDMA precursor synthesis and take valuable part in BB Forum team research of MDMA synthesis new ways.
Equipment and glassware:
- 2 L, 1 L (x2), 0.5 L (x2) and 200 ml (x2) beakers;
- Measuring cylinder for 100 ml;
- 1 L round bottom flask;
- Reflux condenser;
- Magnetic stirrer with heating plate;
- Retort stand and clamp for securing apparatus;
- Laboratory scale (0.1 g-1 kg is suitable);
- Laboratory grade thermometer (20 °C to 200 °C) with flask adapter;
- Funnel;
- Filter paper.
Reagents:
- Potassium hydroxide (KOH) 193.8 g;
- Ethanol (EtOH) 500 ml;
- Piperine 17 g;
- Hydrochloric acid 14% HCl ~500 ml;
- Distilled water;
Procedures
1. KOH 193.8 g and EtOH 500 ml are added into the 1L flask.2. Then piperine 17 g is added.
3. The mixture is stirred until complete dissolution.
4. Then, under the reflux condenser, the mixture is heated at 70-80°С for 10 h.
5. The resulting warm suspension of the formed potassium piperate is drained into a beaker.
6. The suspension's pH is highly alkaline.
7. Next, hydrochloric acid 14% HCl is slowly added to make acidic pH. Avoid overheating.
Note: use appropriate ventilation due to HCl fumes.
8. A portion of water is added until piperic acid is completely precipitated.Note: Glass filters with pore sizes 160 and 100 μm do not filter this sediment, filter with 60 μm pores will be clogged.
9. The precipitated light yellow color piperic acid is filtered through a dense filter paper.10. Piperic acid is dried in a desiccator or under a fan heater to a constant mass.
The acid is a yellow powder with a slight smell of pepper. The yield of piperic acid is 12g or 92.3%.