Author Topic: Biosynth: Homebrewing Ephedrine  (Read 124228 times)

0 Members and 1 Guest are viewing this topic.

Jacked

  • Guest
Biosynth: Homebrewing Ephedrine
« on: July 27, 2001, 05:48:00 AM »
This is a work in progress. It’s by Mobius Bandsaw 
At present I have a fairly good grasp of the means and the end.
You are invited and encouraged to contribute information you may have relating to this subject, we can work together to advance the cause of knowledge.

Shall we begin?

Forward:

When I was given this forum I was also given something of a research assignment.
It seems there is a great deal of interest in the production of ephedrine and pseudoephedrine.    (The forum was called “Homebrewing”)
Both of these products may be obtained in quantity using methods which are in normal practice in industry.
Industrial production of L-PACs uses methodologies which are not altogether removed from the art of distillers of spirits.
While still speaking about theoretical methods of production of alcohols, and products of alcohols, it is hoped that a practical method of production of ephedrine and pseudoephedrine will be achieved which could be employed by the individual
should circumstance find him in need of such capability.
It should be noted from the outset that these methods, recipies, informations, and observations, are not intended to be used by any person.
Further, all persons are hereby advised that use of this information to produce any substance for any illegal purpose is forbidden, and that the author expressly withdraws any permission to read, store, record, or in any way archive this work,
from any person, persons, entity, or organisation, intending to use this information for any illegal purpose.
Any methods discussed here are purely speculative, and for informative and entertainment purposes only, and have not been attempted.
Untrained persons working with devices and substances mentioned here risk serious injury or death.
Production by unlicensed individuals of any substance mentioned or described here could lead to criminal prosecution.

~~~~~~~~~~~~~~~~~~~ 1.~~~~~~~~~~~~~~~~~~~~~
FUN WITH L-PAC production!

Biotransformation processes involving both yeast (Candida utilis) and pyruvate decarboxylase (PDC) for the production of L-phenylacetylcarbinol (L-PAC) from substrates benzaldehyde and pyruvate are an interesting field of study!
L-PAC is an intermediate in the production of ephedrine and pseudoephedrine.
Models for the process with a substrate feeding profile for benzaldehyde will be proposed.
Chiral vicinal aminoalcohols are key building blocks for the production of a number of pharmaceutical products.
Important compounds which may be produced from chiral vicinal aminoalcohol precursors span a range of therapeutic categories and include pseudoephedrine.

Patent US5834261

describes a process that may be employed to produce a broad range of chiral vicinal aminoalcohols, both cyclic and acyclic.
A particularly notable feature of this method is the ability to control the absolute configuration at chiral centers bearing both the amino and alcohol functionality to produce any of the four possible stereoisomers in high stereochemical purity.

Patent US5942644

(issued in August 1999), is related to the process patent described above.

This second patent covers the key intermediates that are involved in the production of chiral vicinal aminoalcohols. These compounds include the hydrazides and hydroxamic acids that are the immediate precursors of chiral vicinal aminoalcohols.
The process for producing chiral vicinal aminoalcohols relies on readily available þ-ketoesters as starting materials.

Examples of þ-ketoesters useful for the production of chiral vicinal aminoalcohols include the inexpensive compounds acetoacetic ester and þ-keto-phenylpropionic acid esters.

Central to this method for the production of these chiral vicinal aminoalcohols is the combination of two key steps, each of which proceeds with a well-defined and controllable stereochemical outcome.

The first step is the stereoselective reduction of the keto group of a þ-ketoester to produce the corresponding þ-hydroxyester.

This reaction is catalyzed by an alcohol dehydrogenase in the presence of a nicotinamide cofactor.

Because of the facile equilibrium between the two enantiomers of a 2-substituted-þ-ketoester in aqueous solution, the interconversion of these two stereoisomers occurs rapidly.

The reduction of the ketone by an alcohol dehydrogenase occurs with a high degree of stereoselectivity, reducing only one of the two ketone enantiomers.
The reduction of the ketone is highly stereoselective for the production of a single alcohol stereoisomer.

so, two chiral centers are generated simultaneously by this enzymatic reaction, and this reaction provides for control of stereochemistry at both the C-2 and C-3 positions of the 2-substituted-þ-ketoester.

NEXT: How earth people do it.

~~~~~~~~~~HOW EARTH PEOPLE DO IT~~~~~~~~~~~~

 If your nitemares never include metalic voices coming over loudspeakers
demanding that you throw out your five gallon plastic buckets and come out with
your hands up, congratulations...you may be on Earth.
Earth people find many wonderful uses for the humble five gallon plastic bucket, as we shall soon see.
 Any earth native who wishes to produce L-PAC at home may discover these utilitarian devices to be worth well more than their wieght in gold.
To produce L-PAC using biosynth methods, one must first decide what will be fermented in the buckets.
In the course of my research I have discovered that the liquid obtained by the crushing, grinding, pressing, and filtering of the common sugar beet is in fact the best possible substance to use for this method due to natural enzyme feeding, but it
is by no means the only one, according to everyones favorite Uncle, even water may be used as a starting point!
After obtaining the liquid to be used, one may wish to fortify it with a bit of brewers sugar.
Into the 4.5 gallons of liquified beet extract one may add about 5 lbs of brewers sugar until the sugar no longer wishes to disolve, the reason for this being the already high sugar content of the extract.
The next requirement is to add yeast. Not just any yeast will do.
For our purposes the strain named Candida Utilis is understood to be best, however, experimentation is encouraged.
Candida Utilis enjoys wide popularity, and may easily be obtained.
The proper addition of yeast is a point of contention.
Many "experts" say that one adds only a small amount, such as say a couple of packets of brewers yeast.
Others state that it is necessary to put in an amount of wieght equal to the added sugar. It would seem to me that a benefit of doing this would be that the process will progress much quicker (three or four days, as opposed to three or four weeks) if
one were to add the larger amount of yeast.
Yeast is expensive if you buy it one package at a time.
Most brewers know how to increase yeast.
Those who do not are again encouraged to purchase a brewers manual detailing the method.

Another required substance is Benzaldehyde.

The production of L-PAC will be directly proportional to the amount of Benzaldehyde used. Returns are expected to be in the range of 60 to 80% the wieght of the added Benzaldehyde.

Once the needed items have been procured one may begin the progress of biosynthesis.

Step one involves mixing the nutrient, which is the liquid, and sugar. Next one adds the yeast to the mixture.

Be careful to avoid contamination of your mixture!

After combining the ingredients, place the top loosely on the five gallon bucket. With the passage of an hour or so one may begin to see the process of fermentation begining, it is felt that the passage of at least 10 hours is needed to allow the fermentation process to fully become active.

After ten hours one must add the benzaldehyde. For this feeding profile the proper amount is calculated to be 60ML.

After adding the Benzaldehyde the fermentation should be left to progress in a cool place away from sunlight. While underway this process also needs to be free of physical shock, such as thumps, and quaking, since this retards the process. If you have a Rock and Roll band and practice in the garage, don't do your biosynth there.

NEXT: IT WORKED! NOW WHAT?

~~~~~~~~~IT WORKED! NOW WHAT?~~~~~~~~~~~~~

Now that your fermentation has completed you have your precurson to ephedrine just floating around in your five gallon bucket.
It's not doing you much good in there is it?
The next thing you want to do is to recover your phenylpropanol which is what the yeast turned the sugars into with the help of the benzaldehyde.
The most direct method of recovery is to use a centrifuge, but few of us have one on hand. A more practical method for the small scale producer is filtration.
Now that you have your filtered liquid it is time to begin extracting the phenylpropanol.
To extract the phenylpropanol, you will need to use a non polar solvent, here you may choose between Acetone, Tolulene, or Xylene (personal preference here is toward acetone).
The about 200ml of NP should be added to the mixture, swirled, then allowed to seperate, then decanted, save it, your goodies are there. Repeat this proceedure three times.
At the end of the third wash you should have your phenylpropanol in solvent.
Next you will need to distill the solvent/phenylpropanol in order to remove the solvent.
Once your solvent is largely gone you will again need to distill, but this time you will need to use vacuum in your distillation process. You will need to pull between 14 and 18 torr and your product will come over as phenylacetylcarbinol at between 105c and 155c.
All that remains to be done is a fairly standard reductive amination, whereupon you will find yourself in possession of pure gak free ephedrine.

~~~~~~~~~~~~~~~~~~~NOTE~~~~~~~~~~~~~~~~~~~
Comments, suggestions, and refinements are all solicited.


~~~~~~~~~~~~~~~REFERENCES~~~~~~~~~~~~~~~~~~

Uncle Fester, SOMM
Shin, H.S. and Rogers, Production of L-PAC from benzaldehyde using partially purified pyruvate decarboxylase.
Rogers, P.L., Shin, H.S. and Wang, Biotransformation for L-ephredrine production.


Benzaldehyde: Artificial essential oil of almond; artificial almond flavor is water,
benzaldehyde and alcohol.
Occurs in kernels of bitter almonds; made synthetically from benzal chloride (C6H5CHCl2)
and lime, or by oxidation of toluene.
Hydrolysing benzal chloride is no challenge, boiling in alkaline water. It's making it, by
chlorinating toluene, and keeping it separated from benzyl chloride, the monochloro
derivative, that's the challenge.
In toluene oxidation, the challenge is to prevent overoxidation to benzoic acid. My ballot
is marked for acidic manganese dioxide, but I have seen chromyl chloride mentioned.
A convenient natural source of benzaldehyde is by hydrolysis of amygdalin. That spelling
challenge is a double glucoside of mandelonitrile, benzaldehyde's cyanide derivative.
Mostly in apricot pits and bitter almonds, also the seeds of peaches and cherries.
In these natural sources is some free benzaldehyde, but most of it is locked in the
amygdalin. But there is an enzyme in the natural seeds, which will hydrolyse the
amygdalin for you, when you let the ground seed material stand in water; glucose,
benzaldehyde, and hydrogen cyanide result.

Posted by--anomolon

This is a link you might want to look at:

http://www.geocities.com/dritte123/ephyeast.html



Be sure to look up these two patents,

Patent US1956950

&

Patent US1962476

.

My intent on posting this information is for others to join in on the positive and see if we as a whole could bring this to a standard in our quest to rid our self’s of the dependance of a pill to produce a product. It should be looked at and responded to in that light... one bee of the Hive,   Jacked

Jacked

  • Guest
Re: Biosynth (homebrewing E)
« Reply #1 on: July 27, 2001, 04:38:00 PM »
Could this thread be moved to the serious chemistry forum. It was a mistake placing it
here I believe. 

Paid in Full

slowhand

  • Guest
Re: Biosynth (homebrewing E)
« Reply #2 on: July 29, 2001, 04:53:00 AM »
Swish is very happy that someone was able to rescue this post from the Zonez. Swish has full intention of giving this some serious experimentation when everything is gathered.

Ololuiqui

  • Guest
Re: Biosynth (homebrewing E)
« Reply #3 on: August 20, 2001, 11:22:00 PM »
This is veerrrrrrry interesting!  ;D  I have just a couple of Qs...

1) You suggest using acetone as the non-polar solvent... wouldnt acetone bee miscible with the sugar beet juice?

2) You use 200mL solvent for each extraction - isnt this far too little for 4.5gallons of solution?

3) Would this work for substituted benzaldehydes?  ;D

4) Is it really necessary to vac-distil the L-PAC before doing a reductive amination?

Many thanks,
Ololiuqui

Rhodium

  • Guest
Re: Biosynth (homebrewing E)
« Reply #4 on: August 21, 2001, 12:59:00 AM »
I have heard that the yields are very low with substituted benzaldehydes.

jim

  • Guest
Re: Biosynth (homebrewing E)
« Reply #5 on: August 22, 2001, 02:36:00 AM »
I refer you to this tid bit of info.
__________________________________
   !!!!  I FORGOT TO QUOTE THAT THIS REACTION IS STRONGLY pH DEPENDENT AND
    BEST PROCEEDS AT A pH OF 8-9. !!!!!

    From Agric. Biol. Chem., Volume 50, yr 1986, page 1261

                       "Reductive C3-Homologation of Substituted Benzaldehydes by
    Fermenting Bakers' Yeast

      ...

      ...  A unique reaction catalyzed by Bakers' Yeast is the reductive  C-C bond formation in
    benzaldehyde that results  in the formation of 1-phenylpropane-1,2-diol [ref 3].  This reaction is
    supposed to involve the attack of pyruvic acid, which is formed from sugars through a well known
    pathway, by benzaldhyde to give phenyl-1-hydroxy-2-propanone [ref 4].  This ketol is considered to
    be reduced by alcohol dehydrogenase of the yeast to give the
    diol.  ...

                       ...

      Reduction of aldehydes by fermenting yeast.  General procedure.  To 50 mL of tap water, 12.5 g
    of dry yeast and 10 g glucose were added, followed by stirring
    at room temperature for 10 minutes.  Then a solution of aldehyde 1 (about 600 mg) in 1 mL of
    ethanol was added to the suspension of  fermenting yeast with stirring.  After 1 hour yeast (6.2 g)
    and glucose (5 g) were added to the reaction mixture, followed by stirring for an additional 3.5
    hours.  The reaction mixture was then  poured into a beaker containing 35 grams of celite and
    extracted with 100 mL of ethyl acetate three times.  The combined organic layer was dried over
    anhydrous Na2SO4.  The solvent removed under  reduced pressure to give an oil consisting of
    benzylic alcohol 3, 1-arylpropane-1,2 diol 3, and in
    some cases, 1-aryl-1-hydroxy-2-propanone 4.  ...

                       Table II.  Yields and Steroselectivities of propanediols (a)
                     
    _____________________________________________________________
                       Substrate______Yield %____...
                     
    ______________________________________________________________
                       H______________30
                       p-OMe__________22
                       p-Me____________28
                       p-Cl____________27
                       p-F_____________26
                       p-NO2__________14
                       o-Me____________7
                       o-Cl_____________32
                       o-F_____________30
                       m-F____________31
                       CF3(e)__________0
                       _________________________
                       (a) Reactions were carried out in tap water at room
    temperature ... (e)  All of the o-, m-
                       p-substituted isomers gave no diols."
_________________
If i remember correctly, the diol can be rearranged to form P2P with H2SO4

Jacked

  • Guest
Re: Biosynth (homebrewing E)
« Reply #6 on: August 22, 2001, 11:45:00 AM »
You suggest using acetone as the non-polar solvent... wouldnt acetone bee
 miscible with the sugar beet juice?

At the point in the procedure that the acetone is used, the sugar beet
juice has been fermented.
The solvent will collect what it is after, and seperate (layer).

You use 200mL solvent for each extraction - isnt this far too little for 4.5gallons of solution?

Most of the 4.5 gallons is junk that you are not interested in. The 200Ml
per extraction is conservative, you may use more if you wish, the only
complication is the added seperation/evaporation time.

Would this work for substituted benzaldehydes?

It would depend on the substitution

Is it really necessary to vac-distil the L-PAC before doing a reductive
amination?

 Yes. Without the vacuum distillation you will not be aminating only the
desired substance. I am unsure what contaminates may reside in the
undistilled form. For safety's sake, I would not skip this step.

Answers were given to these questions by the writer of the original post.

http://crystalninjas.net/jacked/disclaimer.htm

Whizard

  • Guest
Re: Biosynth (homebrewing E)
« Reply #7 on: August 22, 2001, 07:07:00 PM »
In your quotation from the journal you say:
The solvent removed under  reduced pressure to give an oil consisting of
    benzylic alcohol 3, 1-arylpropane-1,2 diol 3, and in
    some cases, 1-aryl-1-hydroxy-2-propanone 4.  ...

 What is the 4. part of the last word? I do not want to assume anything!!!
It also appears that the large excess of yeast is used to allow immediate gratification to the above mentioned experimentalists!

I dunno, but I been told ... You never slow down, you never grow old!

jim

  • Guest
Re: Biosynth (homebrewing E)
« Reply #8 on: August 23, 2001, 04:03:00 AM »
To clarify:

"... benzylic alcohol 3, 1-arylpropane-1,2 diol 3, and in
       some cases, 1-aryl-1-hydroxy-2-propanone 4.  ..."

the 3, and 4 refer drawings of the compounds on diagram not included.

Antoncho

  • Guest
Re: Biosynth (homebrewing E)
« Reply #9 on: September 19, 2001, 07:14:00 PM »
....having read the proc. about getting -propanediol from benzaldehyde, i couldn't help wondering about 2 things:

1) The procedure doesn't mention any sort of pH adjustment - how is pH supposed to get to 9? It also just looks strange - what is the origin of that 1st phrase, the one in CAPS? Jim, you still around? Please, explain!

2) Apart from the pH thing, the whole procedure seems completely identical to l-PAC production!! What is you think that makes the difference?

Antoncho will bee VERY appreciative of any help on this issue, cause SW He Doesn't Even Know just happens to have a kilo of benzaldehyde lying around with no use for it :):):)

Thank you all in advance,

impatiently awaiting
Antoncho

P.S. Dear Moderators, do you really think this thread belongs here? - if mr. Jacked doesn't mind...

foxy2

  • Guest
Re: Biosynth (homebrewing E)
« Reply #10 on: September 20, 2001, 05:05:00 AM »
*****ADVANCES IN BIOCHEMICAL ENGINEERING/BIOTECHNOLOGY*****
Rogers PL  Shin HS  Wang B 
Biotransformation for L-ephedrine production.
In: Adv Biochem Eng Biotechnol (1997) 56:33-59
ISSN: 0724-6145

L-ephedrine is widely used in pharmaceutical preparations as a decongestant and
anti-asthmatic compound. One of the key intermediates in its production is
L-phenylacetylcarbinol (L-PAC) which can be obtained either from plants (Ephedra
sp.), chemical synthesis involving resolution of a racemic mixture, or by
biotransformation of benzaldehyde using various yeasts. In the present review,
recent significant improvements in the microbial biotransformation are assessed
for both fed-batch and continuous processes using free and immobilised yeasts.
From previous fed-batch culture data, maximal levels of L-PAC of 10-12 gl-1 were
reported with yields of 55-60% theoretical based on benzaldehyde. However,
recently concentrations of more than 22 gl-1 have been obtained using a
wild-type strain of Candida utilis.
This has been achieved through optimal
control of yeast metabolism (via microprocessor control of the respiratory
quotient, RQ) in order to enhance substrate pyruvate production and induce
pyruvate decarboxylase (PDC) activity. Processes involving purified PDC have
also been evaluated and it has been demonstrated that L-PAC levels up to 28 gl-1
can be obtained with yields of 90-95% theoretical based on the benzaldehyde
added. In the review the advantages and disadvantages of the various strategies
for the microbial and enzymatic production of L-PAC are compared. In view of the
increasing interest in microbial biotransformations, L- PAC production provides
an interesting example of enhancement through on-line control of a process
involving both toxic substrate (benzaldehyde) and end-product (L-PAC, benzyl
alcohol) inhibition.



Shin, H.S. and Rogers, P.L. (1996) Production of L-PAC from benzaldehyde using partially purified pyruvate decarboxylase (PDC). Biotechnol. Bioeng. 49, 52-62.

Shin, H.S. and Rogers, P.L. (1996) Kinetic evaluation of biotransformation of benzaldehyde to L-PAC by immobilized pyruvate decarboxylase. Biotechnol. Bioeng. 49, 429-436.

This one looks really good, a review article!
Oliver, A. L., Anderson, B. N. and Roddick, F. A. (1999) Factors affecting the production of L-phenylacetylcarbinol by yeast - a case study, Advances in Microbial Physiology, vol 41, pp1-41.

V.B. Shukla and P.R. Kulkarni, (2000) L-Phenylacetylcarbinol (LPAC) : biosynthesis and industrial applications,World J. Microb. Biotech. 16, 499-506 (UK).




Do Your Part To Win The War

Prdy2GO

  • Guest
Re: Biosynth (homebrewing E)
« Reply #11 on: September 24, 2001, 06:27:00 PM »
SWIM translation:

OK all motovation inside starting with 4lbs white sugar and 2-3gallons h2o boiled and allowed to cool then added 1oz of active dry yeaqst (red and yellow jar)
Question is this canditas utilits ? what would work better? Is that super yeast for beer the right stuff?
About ten hours and then 60 ml distalled benzaldehyde was added.
4 days have elapsed and now I am thinking about what to do next?
Thanks


Hum did you get that?

foxy2

  • Guest
Re: Biosynth (homebrewing E)
« Reply #12 on: September 25, 2001, 02:02:00 AM »
Process parameters and reusability of the free cell mass of Torulaspora delbrueckii for the production of L-phenylacetylcarbinol (L-PAC).
AU: Shukla-V-B; Kulkarni-P-R {a}
SO: World-Journal-of-Microbiology-and-Biotechnology.
April, 2001; 17 (3): 301-306..
PY: 2001


The effect of process parameters on the biotransformation of benzaldehyde to L-phenylacetylcarbinol (L-PAC) using a yeast isolate identified as Torulaspora delbrueckii was studied. The maximum yield of L-PAC obtained was (331 mg) per 100 ml biotransformation medium (glucose 3%, peptone 0.6% and at pH 4.5) from 600 mg of benzaldehyde with 8 h of reaction at 30+-2degreeC. Growing the organism in presence of 3% glucose reduced the biotransformation time to 120 min. Addition of 0.6% acetaldehyde (30-35%) lead to an increase in L-PAC yield to 450 mg%. Semi-continuous feeding of benzaldehyde (200 mg) and acetaldehyde (200 mul) four times at 30 min intervals could produce 683 mg of L-PAC/100 ml biotransformation medium. Chiral HPLC analysis of purified L-PAC and PAC-diol showed 99% enantiomeric purity. The cell mass was found to be reusable for biotransformation up to nine times when benzaldehyde and acetaldehyde levels were maintained at (350 mg and 350 mul)-(400 mg and 400 mul). At concentrations from 450 mg and 450 mul to 600 mg and 600 mul, however the cell mass could give efficient biotransformation only during one use.


Based on this you could get up to 100+ grams of L-PAC in a one day 5-gallon fermentation!!

Do Your Part To Win The War

foxy2

  • Guest
Re: Biosynth (homebrewing E)
« Reply #13 on: September 26, 2001, 07:11:00 AM »
I wonder what would happen if you put indolecarboxaldehyde in this fermentation???  Easy AMT?

Would a RP/I reaction reduce indole?

Do Your Part To Win The War

thissuks

  • Guest
Re: Biosynth (homebrewing E)
« Reply #14 on: October 12, 2001, 01:07:00 AM »

both yeast (Candida utilis) and pyruvate
decarboxylase (PDC)




What type of home brewing are these used for?


BISD: Built-in shit detector 

encopo

  • Guest
Re: Biosynth (homebrewing E)
« Reply #15 on: October 13, 2001, 01:48:00 AM »
pardon my stupidity, but:
this biosynth states that it creates l-ephedrine (after
reductive amination of l-pac).
However, upon reduction, won't this yield l-methamphetamine?
Forgive me if I am incorrect, but isn't the l-isomer of
methamphetamine much less effective, and is used in vicks'
inhalers?
Flames welcome.

Don't mind me. I'm mentally ill.

Rhodium

  • Guest
Re: Biosynth (homebrewing E)
« Reply #16 on: October 13, 2001, 10:00:00 AM »
l-ephedrine gives d-methamphetamine, and d-pseudoephedrine gives d-methamphetamine. Seems a little illogical at the first glance, but that is indeed the case.

encopo

  • Guest
Re: Biosynth (homebrewing E)
« Reply #17 on: October 13, 2001, 05:05:00 PM »
yes, thanks rhodium, I realised that after I left and
was reading a doc on catalytic hydrogenation, and it
said (-)-ephedrine and (+)-psuedoephedrine yield
(+)-methamphetamine. I knew d-psuedoephedrine gave us
the right isomer, I assumed it was the same for ephedrine.

I've been looking around for a nice way to get some
benzaldehyde to use in this. looking at the
"phenylacetones.htm" file I found a patent reference
for the production of benzyl chloride by the chlorination
of toluene (it's the same thing as toluene with 1 xtra
Cl on the carbon outcrop).
The process bubbled Cl2 through Toluene, but it also said
that using "bleaching powder" at high temperature with
an acid provides nascent chlorine.
However, the guy who wrote this has a bitch about side
products. Now here is the NICE bit:

"I have discovered, however....,
by heating to a high temperature
an anhydrous mixture of toluene
and bleachin powder, with thorough
commingling, and without the use of
any acid, the chlorination of the
toluene is effected without any of
the disadvantages incident to the
processes above referred to. In
the absence of any added water the
chlorin from the bleaching powder
seems to go directly to produce
benzyl chlorid in the side chain
without attacking the nucleus, even
though the process is carried on in
the presence of iron, as in an
iron vessel"

Hmm. That looks nice. The reaction is pretty much:
Heat toluene to 90'C. Slowly add equal amount (weight)
of Ca(OCl)2 (pool shock), and raise temperature to
100'-105'C, leaving it there 1 hour or until reaction
complete. Settle. Decant of oil.

This oil contains 30-35% benzyl chloride and 65-70%
toluene.
However, We don't want benzyl chloride, do we? We want
BENZAL chloride. The patent goes on to describe that if
sufficient amount of Ca(OCl)2 is added, the toluene is
completely converted to Benzal Chloride and
Benzo Trichloride. Upon boiling in alkaline water, we
get Benzaldehyde and Benzoic acid. Voila.

Hope this will be a good addition to the home-brew-E
method, as many bees don't have that much benzaldehyde
lying around.

Check out the patent:




Don't mind me. I'm mentally ill.

encopo

  • Guest
Re: Biosynth (homebrewing E)
« Reply #18 on: October 13, 2001, 10:58:00 PM »
Sorry you can't see the above. The patent is:
U.S. Pat.#1,280,612

Also, if the concentration of benzaldehyde in synthetic
almond essence is high enough, then the alcohol could
just be boiled off, and the rest plopped into the bucket.

Also, is it possible to get out the L-PAC in a fashion that
does not require vacumn distillation?

Ooooh! Here we go, info on the almond essence:

Bitter Almond oil is a light colourless liquid with a characteristic 'marzipan' scent. It main constituents are benzaldehyde (95%) and prussic acid (3%)."

bitchin! That's an extremely high amount. However, I'm not
convinced that this will be the concentration in OTC almond
essence. Perhaps if "imitation" essence is used, there will
be no prussic acid, as the essence will be made from
benzaldehyde, rather than via almonds. Maybe? Maybe not.

I'll be watching & working with you on this one.



Don't mind me. I'm mentally ill.

encopo

  • Guest
Re: Biosynth (homebrewing E)
« Reply #19 on: October 13, 2001, 11:06:00 PM »
pardon my ever growing list of posts but...
It seems that the strain Candida Utilis is often
one of the organisms responsible for...
VAGINAL YEAST INFECTIONS!
This is really, really, really gross.
Okay, so who's going to be the first person to make
ephedrine from almond essence, vaginal yeast & sugar beets
and then meth from phosphorous from a human skull, and
iodine from stinky ol' kelp & dead fish.

Mmmmm. yummy. You can't get much more ORGANIC with this
organic chemistry.

This is bad. This is very very bad. Vaginal yeast.

Don't mind me. I'm mentally ill.