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Soap
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| Joined: 26 Mar 2005 |
| Posts: 86 |
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2156.08 Points
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bio synth of l-pac, starting off
Thu Jun 23, 2005 6:04 am |
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hello all. swims been reading a lot about how easy it is to aquire large amounts of benzaldhyde and he thinks that hes goign to give it a try.. now there seems ot be many diffrent ways to go from benzaldhyde to (----)amphetamine but the most appealing and otc route he has seen so far seems to be the bio synth of l-pac. there is little information on rhodnium on this subjet, and swims been having troubles finidng info elsewere.
Has anyone ever done this? what were your yeilds? how otc can this be. do diffrent strains of yeast make a huge diffrence? for instance, swim has some high alcohol tolerant yeast from his moonshining days, would this work better than say store bought bread yeast?
the conversion of l-pac to ephedrine looks easy but is it? like ive said swim has yet to find a full write up on this method. thanks all for the help! |
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jackoozzi
specialist
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| Joined: 10 Feb 2005 |
| Posts: 135 |
| Location: Australia |
39384.40 Points
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re: bio synth of l-pac, starting off
Thu Jun 23, 2005 7:05 am |
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If you join the brew forum and pm me for access to a restricted section there is a collection of info there
https://www.synthetikal.com/brewforum/ |
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rennie coombs
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| Joined: 22 Jun 2005 |
| Posts: 2 |
| Location: australia |
58.26 Points
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re: bio synth of l-pac, starting off
Wed Jul 20, 2005 8:17 pm |
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jackoozzi,
Could i see some of the l-pac biosynthesis restricted collection?
I see early procedures gave 8% l-pac but believe latest are around 30% .Have you latest best procedures?
Regds |
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: bio synth of l-pac, starting off
Mon Aug 01, 2005 10:22 pm |
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SWIh would really like to get a first timer's procedure either written or acquired, but has no experience. SWIh can brew beer and wine with no problems. SWIh has read all of the available pdf documentation, but has some trouble with the technical terminology. SWIh is no idiot and has a B.S. degree in a technical field.
SWIh's first idea was to use the brewing equipment that SWIh uses for brewing beer, use bakers yeast instead of brewing yeast, add Benzaldehyde in small concentration, and see what happens.
Is the biobrew/biosynth this simple, or will this most definitely fail?
SWIh isn't looking to maximize yield the first time. He/she just wants to run the procedure, and extract some amount of l-PAC. The process can be optimized, later.
If these basic steps have been taken, can someone point SWIh in the right direction? SWIh hasn't found any write-ups that aren't technical articles, journals, patents, etc. A procedure for those only familiar with brewing alcohol but not biosynthesis would be the goal. |
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java
Consumer
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| Joined: 07 Feb 2005 |
| Posts: 736 |
| Location: The Mexican Republic |
21794.14 Points
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re: bio synth of l-pac, starting off
Mon Aug 01, 2005 10:48 pm |
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| hAzzBEEn ......the formost writiings on the subject hav been submitted by Org. look for his posts in the Hive files , and at the sciencemadness forum.....there is also a good thread in the WD which was visited by many with info .....there is a lot of info , one might suggest you archive it and make a folder that you can later offer as the complete catalog of info on L-PAC .... ....just a thought.......java |
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: bio synth of l-pac, starting off
Mon Aug 01, 2005 11:57 pm |
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I will do that. I have all of the pdf's from the Fermentikal "restricted" area. I understand it for the most part. I have read the old threads at Sciencemadness, but the discussion has been dead for a while. I can't get the WD threads because WD is still down. I even have a L-PAC folder, lol.
I think the next step is for SWIh to go ahead and get the ol' hands dirty. SWIh would be more comfortable if someone said, "this is the way I did it, and it worked... do this or that instead of a standard brewer's fermentation". I guess real scientists are leaders and experimenters, not followers. |
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stooge
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| Joined: 11 Feb 2005 |
| Posts: 56 |
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1401.36 Points
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re: bio synth of l-pac, starting off
Tue Aug 02, 2005 10:54 pm |
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a relating question: the only usable Benzaldehyde it swis's location is a thick fluid said to contain also alcohol (no clue which) and water ... could that be used as is or ... ?
swis will try, but as he has no experience with this the only effect will probably be that it won't work and he won't know why ... |
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: bio synth of l-pac, starting off
Wed Aug 03, 2005 12:57 am |
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What was this benzaldehyde designed for? SWIh questions the purity of his/her Benzaldehyde, too. When it was ordered it was simply labelled "Benzaldehyde", but it is sold for a specific purpose, and purity wouldn't be an issue. If answering the question would be bad for your source, you can PM me about it.
I am serious about finding a doable method for this. Surely it is possible. Brewing is dirt cheap and OTC: water, sugar, yeast, nutrients... adding some Benzaldehyde and maybe some Acetaldehyde, and you're still looking at dirt cheap. Hell SWIh's Benzaldehyde was even semi-dirt-cheap. |
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stooge
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| Joined: 11 Feb 2005 |
| Posts: 56 |
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1401.36 Points
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re: bio synth of l-pac, starting off
Wed Aug 03, 2005 2:13 am |
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no problem, it's simple food additive, if that's the right word - almond arome for baking, and stuff ...
it is labled "contains bitter almond extract, alcohol, water" ... not very detailed, unfortunately.
Just the biggest amounts he found without vegetable oil like all the other brands. To order pure Benzaldehyd is pretty suspicious here for privat persons ...
it is of rather thick consistence, colorless and clear like water. swis guesses alcohol and water is better than vegetable oil, but that's all he can say ... he was about just to start a try with some bottles of this stuff in molasses, water and brewers yeast, but as he isn't able to check what the product is afterwards it seems a little useless to him. how does one know wether if there is some L-PAC in the brew or not??
just one other question: shouldn't also Phenylpropanolamin be doable from L-PAC instead of Ephedrin? |
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: bio synth of l-pac, starting off
Wed Aug 03, 2005 2:26 am |
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| stooge wrote: |
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he isn't able to check what the product is afterwards it seems a little useless to him. how does one know wether if there is some L-PAC in the brew or not??
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I asked the same question over at WD. The answer was no help... can't find the post, now. After the "brew", the l-PAC is extracted with DCM. I guess the DCM could be distilled off to leave the organic part. There should be l-PAC and the by product.. benzyl alcohol, I think. These could probably be separated by distillation or vacuum distillation. I need to check the boiling points, etc. Do you have a good source for such info?
Yes, PPA is doable from l-PAC. In one post that I read (I think at Sciencemadness) it was indicated that PPA would be easier than ephedrine. I think l-PAC => Ephedrine requires Methylamine, while l-PAC => PPA does not. It may not be exactly the same reaction, though. IIRC, the l-PAC can be reduced with an Al/Hg with methylamine to yield l-ephedrine.
Would PPA be more desireable that ephedrine? Does SWIS know anything about 4-MAR synth. SWIhAzzBEEn would love that information. Where are the good write-ups that I've heard about at WD-almost loaded?
Does SWIy have distillation equipment? The Benzaldehyde can be purified/separated by vacuum distillation. I have a write-up on purifying Benzaldehyde, somewhere. I will try to dig it up. |
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stooge
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| Joined: 11 Feb 2005 |
| Posts: 56 |
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1401.36 Points
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re: bio synth of l-pac, starting off
Wed Aug 03, 2005 2:40 am |
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swim will get some distillation equipment as soon as possible, but vacuum ... ugh ...
will look after the boiling points, but as he doesn't know what kind of alcohol they mixed in it might be a problem. Swim hopes it might work without purifying as alcohol will be build anyway while fermentation and water is in the mix also, so ... but that might be pure wishfull thinking.
on the other hand: he still got a 20 year old bottle of 250ml of Benzaldehyd, a third of it is full with solid benzoic acid ... could this be "reactivated" again, somehow?
somewhere swim read about the smell of L-PAC and he understood it like it would stink terrible ...
but, i guess anything with sugar and brewers yeast might smell somehow mean after a few days
the bp for benzyl alcohol seems to be 205 C, couldn't find l-Phenylacetylcarbinol yet. did swim even spell it right? |
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: bio synth of l-pac, starting off
Wed Aug 03, 2005 8:19 pm |
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Once SWIy has distillation equipment, the vacuum part is easy. That is assuming that SWIy get distillation equipment with ground glass joints. Water aspirators that can screw into your water faucet are $20 or less. A used vacuum pump can be acquired for higher vacuums. SWIh still needs to re-up his/her lab equipment, too, as he/she disposed of most of it some time ago.
Alcohol should boil at a much lower temp than Benzaldehyde. Do you know where to look up this data if it's not handy? The Alcohol could be boiled out at the least (if the heat doesn't disturb the Benzaldehyde). I'm not sure about the benzoic acid. Does that precipitate over time from benzaldehyde? Couldn't SWIy just decant some of the benzaldehyde and use that, for now?
Have you brewed before? The smell of regular brewing is not very strong/loud. Some find it quite pleasent. For all I know, L-PAC might smell like shit. Again, a good source for such information would be nice.
About SWIy's food product benzaldehyde, you could request the MSDS from the manufacturer (do they have MSDS's for food products?). It should have some useful information such as the type of alcohol present. It shouldn't matter as the alcohol should boil at a lower temperature, anyway.
I think SWIy spelled it right. I prefer the term hydroxyphenylacetone. I read somewhere that phenylacetylcarbinol was originally named incorrectly, but the name stuck. It won't be long before were talking about HP2P or hydroxy-P2P. |
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: bio synth of l-pac, starting off
Fri Aug 05, 2005 7:36 pm |
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I have been looking for the physical properties of L-PAC (Other names: Phenylacetylcarbinol, 1-Phenylacetylcarbinol, 1-Hydroxy-1-phenylacetone, 1-hydroxy-1-phenyl-2-Propanone, NSC404583, 90-63-1). I checked in the CRC Handbook of Chemistry and Physics and there was no listing for 2-Propanone, 1-hydroxy-1-phenyl-.
Can someone check the Merck Index for the properties?
I only have the CRC Handbook.
Any suggestions for finding this information? |
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: bio synth of l-pac, starting off
Sat Aug 06, 2005 11:38 pm |
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I found the properties, but only in a thread at Sciencemadness. The properties are quoted below and found in the following thread in a post by Organikum:
Hydroxylamine NH2OH Uses (and Production)
| Quote: |
CAS 90-63-1 (1-hydroxy-1-phenyl-2-propanone)
Formula: C9H10 O2
Composition: C, 71.98; H, 6.71; O, 21.31
Mol. Weight: 150.1745
Exact Mass: 150.06808
1-hydroxy-1-phenylacetone, aka Acetylphenylcarbinol, boils at 205-7° C at atmospheric pressure, 135-7° C at 24 mm Hg, 140-5° C at 11 mm Hg and 66° C at .2 mm Hg It's miscible with most organic solvents.
C6H5CHOHCHOCH3
1-hydroxy-1-phenyl-2-propanone
1-hydroxy-1-phenylpropanone
1-phenylpropan-1-ol-2-on (phenylpropanolon) -> old german
phenylpropanolone
1-phenyl-2-ketoalcohol-(1)
1-phenyl-propanol-1-one-2
PAC
Acetylphenylcarbinol
phenylacetyl carbinol
1-phenylpropan-1-ol-2-one
1-hydroxy-1-phenylacetone
1-phenyl-1-hydroxyacetone
Benzacetoin (german)
Funny:
The mostly referred form is laevo-phenylacetylcarbinol aka
l-phenylacetylcarbinol aka
l-PAC aka
L-PAC aka
R-PAC (thats a good one hey!)
because of:
(R)1-hydroxy-1-phenyl-2-propanone is correct for laevo-phenylacetylcarbinol.
Even more funny is that phenylacetylcarbinol is WRONG as this describes an isomer - but as Neuberg and Hirsch who discovered the stuff made this mistake in their first publications (corrected it lateron) the name is still used.
Do you now know why I HATE chemists?
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: bio synth of l-pac, starting off
Thu Aug 11, 2005 1:38 am |
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I found an old write-up that could be helpful for biotransformation beginners. It is actually some posts made at the Hive.
| Organikum wrote: |
Organikum (Hive Bee)
12-11-02 10:10
No 388449
plain benzaldehyde to hydroxyphenylacetone
How benzaldehyde is transformed to hydroxyphenylacetone:
To a 4 liter mixture containing sterile tap water, 400 gram molasses and 2000 ml brewers wort at 32°C in a usual fermenter 250 gram wet bakers yeast were given. Fermentation started. After one hour 3 gram MgSO4, 8 gram KH2PO4 and 20 gram (NH4)2PO4 were added and ph was adjusted at 4,7 by adding diluted H3PO4. This was allowed to cool down to 25°C. 35ml benzaldehyde in EtOH were added followed by 40 ml acetaldehyde in H2O. Two droppers were installed to drop in 40 ml benzaldehyde and 50 ml acetaldehyde during the next 4 hours. The fermentor was aerated and stirred during the whole procedure.
After 8 hours the yeast was filtered out and the water extracted with petrolether using a perforator. The extraction lasted 12 hours then the petrolether was boiled away and collected for reuse. The remaining sluggish brownish liquid substance, about 130 ml was vacuum distilled and the fraction coming over between 120° to 150°C @ 18 torr was collected. It was about 80 ml which were processed further by an Al/Hg reductive alkylation shameless copied from MaDMAx. Thanks Max! The result of 25 gram ephedrine is mostly to blame on slappy handling, low experience, not éxtracting the yeast and 47.123 more small mistakes adding up. But for it was l-ephedrine, (TLC comparism to a probably clean sample, melting point, taste...) the reaction before has to have produced hydroxyphenylacetone and that was what was to proove. It was the first run, a "proove of principle" and for this it was more than a success.
Important is heavy aeration with sterile air and permanent ph control with adjusting at <5,3. Doing some test batches with yeast only is adviced. The whole procedure is certainly more related to brewing than to chemistry what is not negative IMHO. Later runs gave better results, literature claims >70% on benzaldehyde and I think that thats realistic, >50% should be reachable for everyone with some excercise.
This works on substituted benzaldehydes also as I believe also I don´t know if the dehydroxylation is a problem then. PPA is easily made and perhaps a more direct way to 4-MAR is possible? I don´t know.
ORGY
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| Organikum wrote: |
Organikum (Hive Bee)
12-11-02 17:38
No 388593
patent and brewers wort
The patent Patent US3338796 shows the possibility of using the described procedure on substituted benzaldehydes. Also an alternative fermentation medium is disclosed and a easy way for finding the right strain of yeast.
The synthesis described by me before is the best yielding known (the yields I got first time don´t count). Only if extracted and purified enzymes are used higher yields are propagated - up to 99%.
The "brewers wort" is here the wort as prepared for brewing a lager beer up to the point where the hops would be added. No hops and more important no boiling. The temperature of the malt (and wort) must never exceed 78°C. Or your coenzymes are gone. And for providing these coenzymes on a natural and cheap way the wort is used. Concentration of the wort should be this that it contains about 18% fermentable saccharose. A look for beer brewing answers most technical questions on fermentation, aeration, saccharose concentration, sterilisation.......
The used molasses should be made from sugar beets and contain about 50% sugar.
ORGY
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