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Owsley's wife and James Fadiman (inventor of microdosing) don't seem to approve of MDMA

Sansert said:


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The Nichols protocol—formally published by David E. Nichols' research group in the Journal of Medicinal Chemistry (1986)—is the gold-standard literature method for the classical resolution of racemic MDA into its individual enantiomers, (S)-(+)-MDA and (R)-(-)-MDA. [1]
Instead of mandelic acid, the method employs malic acid isomers to achieve precise fractional crystallization. The protocol involves two separate branches to isolate both enantiomers cleanly.

Phase 1: Isolation of (S)-(+)-MDA​

This phase selectively crystallizes the (S)-enantiomer using (R)-(-)-malic acid (also known as D-malic acid).
  1. Dissolution: Racemic MDA free base is dissolved in a minimum amount of boiling absolute ethanol or a hot mixture of ethanol and water.
  2. Acid Addition: An equimolar amount of (R)-(-)-malic acid is dissolved and added to the hot MDA solution.
  3. Crystallization: The mixture is allowed to cool slowly to room temperature, then chilled in a refrigerator overnight. The (S)-(+)-MDA • (R)-(-)-malate salt preferentially forms a crystalline precipitate, leaving most of the (R)-MDA salt dissolved in the liquid (mother liquor).
  4. Filtration: The crystals are filtered out. The liquid mother liquor is set aside and saved (it is heavily enriched with the remaining (R)-MDA).
  5. Purification: The collected crystals are recrystallized from ethanol until a stable, constant melting point and constant optical rotation are achieved, ensuring high enantiomeric excess (% ee).
  6. Basification: The pure crystals are dissolved in water, made strongly alkaline with sodium hydroxide (NaOH), and the freed (S)-(+)-MDA base is extracted using an organic solvent (such as ether or dichloromethane) and evaporated.

Phase 2: Isolation of (R)-(-)-MDA​

This phase recovers and purifies the opposite enantiomer from the saved liquid.
  1. Recovery: The mother liquor saved from Phase 1 is evaporated to dryness.
  2. Basification: The residue is dissolved in water, treated with a strong base (NaOH), and extracted to recover the crude, free-base MDA (which is now highly enriched with the (R)-enantiomer).
  3. Chiral Switching: This recovered base is dissolved in boiling absolute ethanol, but this time an equimolar amount of (S)-(+)-malic acid (L-malic acid, the naturally occurring form) is added.
  4. Crystallization: The solution is allowed to cool slowly. Because the remaining base is mostly (R)-MDA, it now forms a less-soluble crystalline salt with the (S)-malic acid, precipitating cleanly as (R)-(-)-MDA • (S)-(+)-malate.
  5. Final Isolation: The crystals are filtered, recrystallized for purity, and basified using the same extraction steps to yield pure (R)-(-)-MDA free base.

Summary of Salt Affinities​

(S)-(+)-MDA(R)-(-)-Malic Acid (D-malic)Less-soluble precipitate (Crystallizes first)
(R)-(-)-MDA(S)-(+)-Malic Acid (L-malic)Less-soluble precipitate (Crystallizes from recovered mother liquor)
[th]
Target Enantiomer​
[/th][th]
Chiral Resolving Agent Used​
[/th][th]
Salt Formed​
[/th]​
 
Didgital said:
hey so how can one measure optical rotation?
without a polarimeter i mean.
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Aside from a 3d printer DIY or student polarimeter (often called a manual or Laurent's half-shade polarimeter) is a classic, entry-level lab instrument designed specifically for schools and colleges, chiral TLC

you can buy Chiral TLC plates (or treat standard plates with a chiral selector like cyclodextrin)

[The stationary phase on the plate is chemically modified to be chiral. One enantiomer will bind tighter to the plate than the other, causing them to separate into two distinct spots as the solvent moves up]

[[You can impregnate standard, cheap TLC plates by dipping or spraying them with a solution of a copper salt and an optically active amino acid.

Common Recipe: A solution typically consisting of copper(II) acetate and L-proline (or N,N-dimethyl-L-phenylalanine) in a solvent like water/methanol is used to coat standard plates. Once dried, these plates function on the same ternary complexation principle as commercial options at a fraction of the cost.]]
 
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Sansert said:
Aside from a 3d printer DIY or student polarimeter (often called a manual or Laurent's half-shade polarimeter) is a classic, entry-level lab instrument designed specifically for schools and colleges, chiral TLC

you can buy Chiral TLC plates (or treat standard plates with a chiral selector like cyclodextrin)

[The stationary phase on the plate is chemically modified to be chiral. One enantiomer will bind tighter to the plate than the other, causing them to separate into two distinct spots as the solvent moves up]

[[You can impregnate standard, cheap TLC plates by dipping or spraying them with a solution of a copper salt and an optically active amino acid.

Common Recipe: A solution typically consisting of copper(II) acetate and L-proline (or N,N-dimethyl-L-phenylalanine) in a solvent like water/methanol is used to coat standard plates. Once dried, these plates function on the same ternary complexation principle as commercial options at a fraction of the cost.]]
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Looks like natural malic resolves the tripping form of mda ....
 
It's like people miss the point. You can produce optically pure MDA from PMK via a chiral synthesis.

Reductive amination with the isomer of α-methylbenzylamine you seek then debenzylation.

As used to produce dexamphetamine since the 1960s.

I would assume with PMK being the pinch-precursor, a chiral synthesis would be far more efficient on almost every metric. If you can obtain cheap PMK in unlimited amounts, I would still imagine the method used to make dexamphetamine would still be preferred as if nothing else, you don't get two isomers - just the one you make.
 
4DQSAR said:
It's like people miss the point. You can produce optically pure MDA from PMK via a chiral synthesis.

Reductive amination with the isomer of α-methylbenzylamine you seek then debenzylation.

As used to produce dexamphetamine since the 1960s.

I would assume with PMK being the pinch-precursor, a chiral synthesis would be far more efficient on almost every metric. If you can obtain cheap PMK in unlimited amounts, I would still imagine the method used to make dexamphetamine would still be preferred as if nothing else, you don't get two isomers - just the one you make.
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The palladium balloon hydrogenation trick?
Just know the surface of the catalyst gets clogged and needs to be cleaned for recycling re-use.
 
US4000197A - wellwillyyalookatthastname.

But in fact Allan and Hanburys had been using the route since 1964 (and in fact the US patent cites their work).

Back in the 1960s it was more practical to NOT to patent a method since that only protects for 20 years but to employ a simple need-to-know basis since back then pharmacutical companies were led by medicinal chemists, not amoral psychopaths who saw industrial espionage as a valid route so A&H just made the product cheaper than anyone else and the few staff who understood the route signed NDAs back when they were enforcable.

When evidence of having broken an NDA rendered a person unemployable (at best) and sometimes in actual legal trouble.
 
4DQSAR said:
US4000197A - wellwillyyalookatthastname.

But in fact Allan and Hanburys had been using the route since 1964 (and in fact the US patent cites their work).

Back in the 1960s it was more practical to NOT to patent a method since that only protects for 20 years but to employ a simple need-to-know basis since back then pharmacutical companies were led by medicinal chemists, not amoral psychopaths who saw industrial espionage as a valid route so A&H just made the product cheaper than anyone else and the few staff who understood the route signed NDAs back when they were enforcable.

When evidence of having broken an NDA rendered a person unemployable (at best) and sometimes in actual legal trouble.
Click to expand...
Have interacted with doctor dave for some time to prove my innocence, and seeing that patent, knowing he has devised a 13 or 14 analog from that recent joel smith synthesis of lysergic, and joel smith being a consultant and his financial situation due to various marriages, likely will seek joel and him to patent a more proproietary synth, and not make a hill of beans, he best hope you buy his books. His first is a stab in the science fiction genre, soon to be published ....
 
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