# MD-P2P Synthesis using a TEMPO Oxidation



## Isotaffy (Mar 23, 2022)

My thoughts were Safrole to MP-P2Pol with Sulfuric Acid and Water
MP-P2Pol to MP-P2P with TEMPO, NaBr, and NaClO in Methylene Chloride/Water

I for one hate wacker oxidation, so figured I could try this instead.
Step 1 Hydration









Step 2 Tempo Oxidation



(MD-P2P)


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## halohydrin

Oxidation with TEMPO and hypochlorite can be done on two phase system as you mentioned. Some phase-transfer catalysts like TBA salts can help.
But since it's a secondary alcohol, I assume you can use any oxidizer which can oxidize primary alcohols to aldehydes/acids, like dichromates, permanganates... unless it breaks down the methylenedioxy ring.


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## 84%

The new _MAPS cGMP_ process publication describes that TEMPO oxidation in "Stage 2: Oxidation to 1-(3,4-Methylenedioxyphenyl)-propan-2-one" of "Fully Validated, Multi-Kilogram cGMP Synthesis of MDMA"

Note that "1-(3,4-Methylenedioxyphenyl)-propan-2-one" is just another name for *piperonyl methyl ketone* (*MDP2P* or *PMK*).

If you are considering that path, you may as well try Stage 1 from the same publication (ACS Omega 2022, 7, 900−907).


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## 84%

84% said:


> The new _MAPS cGMP_ process publication describes that TEMPO oxidation in "Stage 2: Oxidation to 1-(3,4-Methylenedioxyphenyl)-propan-2-one" of "Fully Validated, Multi-Kilogram cGMP Synthesis of MDMA"
> 
> . . .
> 
> If you are considering that path, you may as well try Stage 1 from the same publication (ACS Omega 2022, 7, 900−907).



84%That was the PDF URL, which does not always load properly.

Better use the /doi/10.1021/acsomega.1c05520 path.
Or try /10.1021/acsomega.1c05520 on DOI ORG instead.

On Stage 1 idea: it uses _5-bromo-1,3-benzodioxole_ instead of safrole as the starting chemical.

From the paper: _"We identified 5-bromo-1,3-benzodioxole (*11*), which does not appear on any geopolitical entity’s list of controlled substance precursors, as a useful starting material for our synthesis. The 1,3-benzodioxole moiety appears in a variety of natural products, including oils, (26) spices, (27) and traditional plant-based medicines. (28)"_


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