MD-P2P Synthesis using a TEMPO Oxidation
- Thread starter Isotaffy
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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.
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.
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).
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).
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)"
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)"