Anyone ever try the Bayer-villager route to P2P?

american gopnik

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I’ve seen articles about it on the web yet have read no actual write-ups or results of actual synthesis.
 

OTC_HomeChemist

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Yes - I did plenty of times.

The first step the acid catalyzed aldol condensation is easy and pretty good yields of the intermediate can be achieved.

Now the baeyer villiger Oxidation step is something I've been working on for a long time by now, trying all sorts of different catalysts and reagents. If you have access to something like commercial 40% peracetic acid solution (which I only can get once in a while and only in Limited amounts) then it's an easy and good route to P2P.

Also If you do have access to 30% hydrogen peroxide solutions its still a good route for smaller scale production.

If you're Just looking at producing small amounts of high quality P2P and Not worried about some effort then I guess its one of the best ways when you don't have access to restricted chemicals since everything you need can be bought otc or be produced in a proper Lab setting.

If you have any questions regarding any of the steps I am Sure i can Help. Also got plenty of footage/Pics to illustrate the process.
 

loadingST

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Yes - I did plenty of times.

The first step the acid catalyzed aldol condensation is easy and pretty good yields of the intermediate can be achieved.

Now the baeyer villiger Oxidation step is something I've been working on for a long time by now, trying all sorts of different catalysts and reagents. If you have access to something like commercial 40% peracetic acid solution (which I only can get once in a while and only in Limited amounts) then it's an easy and good route to P2P.

Also If you do have access to 30% hydrogen peroxide solutions its still a good route for smaller scale production.

If you're Just looking at producing small amounts of high quality P2P and Not worried about some effort then I guess its one of the best ways when you don't have access to restricted chemicals since everything you need can be bought otc or be produced in a proper Lab setting.

If you have any questions regarding any of the steps I am Sure i can Help. Also got plenty of footage/Pics to illustrate the process.
OTC_HomeChemistHave you ttried oxone ?
 

Cbison

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Yes - I did plenty of times.

The first step the acid catalyzed aldol condensation is easy and pretty good yields of the intermediate can be achieved.

Now the baeyer villiger Oxidation step is something I've been working on for a long time by now, trying all sorts of different catalysts and reagents. If you have access to something like commercial 40% peracetic acid solution (which I only can get once in a while and only in Limited amounts) then it's an easy and good route to P2P.

Also If you do have access to 30% hydrogen peroxide solutions its still a good route for smaller scale production.

If you're Just looking at producing small amounts of high quality P2P and Not worried about some effort then I guess its one of the best ways when you don't have access to restricted chemicals since everything you need can be bought otc or be produced in a proper Lab setting.

If you have any questions regarding any of the steps I am Sure i can Help. Also got plenty of footage/Pics to illustrate the process.
OTC_HomeChemistI need help with this reaction. I can’t even go past the first step of obtaining MPB crystals. I would like to obtain the MPB crystal without performing the vacuum distillation.

I gas my MEK + Benzaldehyde, allow it sit for 48hrs then I decant bottom layer. Brown layer is washed with water & then NaHco2 solution until neutral. Brown organic oil is dissolved in ethanol and placed in freezer.

After long hours in the freezer there is still no visible sight of crystal. I have tried dipping a from spoon still no crystal. I need help to get MPB crystals.

Do I obtain crystal formation by evaporating some of the solvent until saturation and cool?
 

loadingST

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I dont know can i mention another sites but actualy plenty of people have done it and its not so hard, i only fear you shoud chose good oxidation that wont explode if lose control !
 

OTC_HomeChemist

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Yes I have tried Oxone and I'm a big fan of it since its rather cheap and can be bought at any Hardware Store but I prefer it for epoxidations especially with acetone/dmdo for producing substituted P2P derivatives..

The baeyer Villiger Oxidation with Oxone has a few drawbacks that I am still trying to find a good way to work around but have not managed to yet.... The yields are low and both DMF and Acetonitrile which are good solvents or co solvents for this reaction are Not easy to get for me and using aq. solutions does not Work Well and requires a large molar excess of oxone and since the molar Mass of oxone is pretty large you will need huge amounts of it which makes the work up quite a bitch.
 

OTC_HomeChemist

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As of now for me the best OTC Route to P2P is still phenylalanine to phenylacetonitrile to phenylacetic acid and then a Cross ketonization with glacial acetic acid using FE/FESo4 in high boiling solvents at about 250 degrees celsius. Of course a Tube furnace with manganese or other catalysts works well too but I don't own a Tube furnace and my DIY tube furnace is still unser construction ... Since i don't know when. The dry distillation of Calcium or Magnesium salts works too but its a fucking mess to clean it up and the yields are not really great either...
 

loadingST

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Nowadays any plain p2p method is almost not worth it with the new glycidate prices and accesability throw europe/moscow/usa warehouses.
And for producing substituted phenylacetones preparing the glycidate yourself is not much work
 

OTC_HomeChemist

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Yes you are absolutely right - when it comes to profit and Industrial scale production everyone is using stuff like bmk glycidate... But I love Chemistry and doing synthesis with OTC reagents.
 
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