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You don’t want to be fooled by videos on the forum again, do you? I spent more than a year to successfully make the real process D-methamphetamine hydrochloride
No remarks are uniform at room temperature and pressure
Written by myself
1. Prepare raw materials
20ml P2P
100ml 20% methylamine methanol solution
4g NabH4
1/3 RM 3A molecular sieve (silicon dioxide)
Glacial acetic acid
HCI (concentrated hydrochloric acid)
Sodium hydroxide
Dichloromethane
D-tartaric acid
Anhydrous magnesium sulfate (anhydrous sodium sulfate)
Ether
Ethanol (isopropanol)
2. Generate imine
Add the methylamine methanol solution and P2P to the flask containing molecular sieves, shake evenly, seal and let stand for 6 hours to generate the imine intermediate.
3. Amination reduction
Prepare a container and pour NaBh4 into it. Dissolve it completely in methanol and then pour in the molecular sieve. Add 1 drop of NaBh4 methanol solution per second to the imine intermediate in an ice bath below 10 degrees and add a trace amount of glacial acetic acid. After all the NaBh4 has been added, remove the RM from the ice bath for reductive amination. Do not cover the bottle too tightly and stir for 2 hours to generate methamphetamine.
4. Acidification and evaporation
After removing the molecular sieve, add hydrochloric acid until the pH value of RM is 3, heat and evaporate until the boiling point is close to 100, then add appropriate amount of water and evaporate to the boiling point of 100 to ensure that the methanol is completely removed.
5. Acid-base extraction
RM was poured into a separatory funnel, dichloromethane was added, shaken, and the organic layer was discarded. The aqueous phase was retained, sodium hydroxide was added to a pH value of 12, and then poured into a separatory funnel. New dichloromethane was added to remove the aqueous phase, and the dichloromethane was concentrated and washed with water (twice). After drying with anhydrous magnesium sulfate, a pure free methamphetamine dichloromethane solution was obtained.
6. Steam distillation
After evaporating dichloromethane, use steam to distill out all the free methamphetamine, pour all the liquid in the receiving bottle into the separatory funnel, let it stand and separate the layers, discard the water phase, and obtain pure free methamphetamine
7. Right-handed splitting
Dissolve 6g of D-tartaric acid in the minimum amount of ethanol, heat to boiling, pour into a beaker containing 20g of free methamphetamine, stir evenly while hot, let it stand and crystallize at the bottom, and extract the free D-methamphetamine on the upper layer with ether
8. Acidification crystallization
Add anhydrous magnesium sulfate to dry the free D-methamphetamine extracted with ether, filter out the desiccant, and then introduce hydrogen chloride gas to a pH of 6. Heat and evaporate until it is nearly dry and let it stand and crystallize, which is D-methamphetamine hydrochloride.
No remarks are uniform at room temperature and pressure
Written by myself
1. Prepare raw materials
20ml P2P
100ml 20% methylamine methanol solution
4g NabH4
1/3 RM 3A molecular sieve (silicon dioxide)
Glacial acetic acid
HCI (concentrated hydrochloric acid)
Sodium hydroxide
Dichloromethane
D-tartaric acid
Anhydrous magnesium sulfate (anhydrous sodium sulfate)
Ether
Ethanol (isopropanol)
2. Generate imine
Add the methylamine methanol solution and P2P to the flask containing molecular sieves, shake evenly, seal and let stand for 6 hours to generate the imine intermediate.
3. Amination reduction
Prepare a container and pour NaBh4 into it. Dissolve it completely in methanol and then pour in the molecular sieve. Add 1 drop of NaBh4 methanol solution per second to the imine intermediate in an ice bath below 10 degrees and add a trace amount of glacial acetic acid. After all the NaBh4 has been added, remove the RM from the ice bath for reductive amination. Do not cover the bottle too tightly and stir for 2 hours to generate methamphetamine.
4. Acidification and evaporation
After removing the molecular sieve, add hydrochloric acid until the pH value of RM is 3, heat and evaporate until the boiling point is close to 100, then add appropriate amount of water and evaporate to the boiling point of 100 to ensure that the methanol is completely removed.
5. Acid-base extraction
RM was poured into a separatory funnel, dichloromethane was added, shaken, and the organic layer was discarded. The aqueous phase was retained, sodium hydroxide was added to a pH value of 12, and then poured into a separatory funnel. New dichloromethane was added to remove the aqueous phase, and the dichloromethane was concentrated and washed with water (twice). After drying with anhydrous magnesium sulfate, a pure free methamphetamine dichloromethane solution was obtained.
6. Steam distillation
After evaporating dichloromethane, use steam to distill out all the free methamphetamine, pour all the liquid in the receiving bottle into the separatory funnel, let it stand and separate the layers, discard the water phase, and obtain pure free methamphetamine
7. Right-handed splitting
Dissolve 6g of D-tartaric acid in the minimum amount of ethanol, heat to boiling, pour into a beaker containing 20g of free methamphetamine, stir evenly while hot, let it stand and crystallize at the bottom, and extract the free D-methamphetamine on the upper layer with ether
8. Acidification crystallization
Add anhydrous magnesium sulfate to dry the free D-methamphetamine extracted with ether, filter out the desiccant, and then introduce hydrogen chloride gas to a pH of 6. Heat and evaporate until it is nearly dry and let it stand and crystallize, which is D-methamphetamine hydrochloride.