Synthesis of ephedrine from propiophenone

[G.Patton]

Is it viable ti grow and extract ephedra plant what scale and what chemicals would be used and is this the only synthasis

thcmanI'll make a topic about extracting ephedrine from plants soon

 

[gmo]

I'll make a topic about extracting ephedrine from plants soon

G.PattonHey G.patton,Can I use iodine as a halogen substitute for this reaction? And And HBr/hydrogen peroxide can be used instead of bromine?

 

[G.Patton]

Hey G.patton,Can I use iodine as a halogen substitute for this reaction? And And HBr/hydrogen peroxide can be used instead of bromine?

gmo

Can I use iodine as a halogen substitute for this reaction?

Yes

And And HBr/hydrogen peroxide can be used instead of bromine?

I think yes

 

[Sonnettales]

THEORY OF SYNTHESIS OF EPHEDRINE.

The mechanism of these reactions is well known:
- at the first stage, bromine is attached to propiophenone in benzene, alpha-bromine-propiophenone is obtained;
- at the second stage, bromine is replaced by an amino group, cathinone is obtained (if ammonia is taken as an amine) or methcathinone (if methylamine is used);
- reduce sodium borohydride to phenylpropanolamine (PPA) or ephedrine.
This article describes the synthesis and isolation of ephedrine.

PREPARATION OF ALPHA-BROMINE-PROPIOPHENONE FROM PROPIOPHENONE AND BROMINE.

To a solution of 30.8 ml (0.234 mol, 31.4 g, MW = 134.2) of propiophenone in 120 ml of benzene in a liter flat-bottom flask closed with a reverse refrigerator (running water is not needed), add drop by drop 12.0 ml (0.234 mol, 37.4 g, MW = 159.8) bromine at such a speed that the mass has time to discolor (first add a few drops, wait until it discolors, if this does not happen, the mass is slightly heated). The reaction is exothermic, the addition should be made at such a pace that the temperature does not exceed 35...40 degrees. As the bromine is added, the color becomes slightly yellowish, an ominous kind of smoke spreads from the flask. It's the most tear gas!

After adding all the bromine, the solution is stirred for another 30 minutes, after which the alkalis' solution is carefully added until the foaming stops. In this case, the mixture is slightly heated, and the color is much lighter. Immediately add about 100...200 ml of water, all thoroughly mixed (washed), the water layer (bottom) is separated and discarded, benzene solution of alpha-bromine-propiophenone is used in the second stage in the form in which it turned out. The yield of the product, if you allocate - about 95%.

View attachment 605
SYNTHESIS OF METHCATHINONE.

In a flask with a benzene solution of alpha-bromine-propiophenone, 50 ml of water is added (as an option - not fully select water from washing after the first stage) and within twelve hours, in three to four doses - an aqueous solution of methylamine. Methylamine is enough 1.5...2 equivalent (with these tabs - about 0.4 mol), so the amount is as follows: 40 ml of a 40% solution or 50 ml of a 30% solution. If there is no aqueous methylamine, then instead of water, an aqueous solution of methylamine hydrochloride taken in an amount of 27 g (0.4 mol, MW = 67.5) is poured, and in the reaction process an aqueous solution of alkalis is added: 16 g (0.4 mol, MW = 40.0) NaOH or 22.5 g KOH (0.4 mol, MW = 56.1), taken equimolarily with methylamine hydrochloride.

All the reaction time, the mixture is stirred so that the layers do not separate, while the flask must be closed with a cork to prevent the leakage of methylamine. The temperature is maintained slightly above the room temperature, about 30 degrees. At the same time, the color slowly changes to a more yellow, at the end acquiring orange shades. After this time, the cork is replaced with a reverse refrigerator, an aqueous solution of 10...12 g of NaOH (or 14...16 g of KOH) is added, and the mixture is heated once to 70 degrees. In this case, the alkalis displaces excess methylamine, the color becomes more saturated, the solution is no longer a lacrimator.

The solution is cooled, the water layer (bottom) is separated and thrown away. The benzene solution is washed once with a weak aqueous solution of table salt and once with water taken approximately by the volume of benzene, and sent, in the form in which it turned out, to the next stage of the process. Those who wish can allocate methcathinone.

View attachment 606
PREPARATION EPHEDRINE FROM EPHEDRONE (METHCATHINONE).

In the benzene solution of methcathinone, obtained at the previous stage, with intensive stirring in small portions, add 18 g (0.476 mol, MW = 37.8) of carefully crushed sodium borohydride (NaBH4). When adding each portion after about 5 to 10 minutes, exotherm and foaming begin, so the addition is carried out slowly, taking into account this factor. When the addition is finished, the flask is closed with a reverse refrigerator and the resulting suspension is left to stir intensively at room temperature throughout the day. At the end, the solution is heated once to 30...50 degrees, kept at this temperature for three hours and cooled. The color of the mixture remains unchanged for a long time, at the end it becomes lighter, orange shades disappear.

A concentrated aqueous alkalochi solution (KOH or NaOH) is added to the mixture to facilitate the filtration of borohydride suspension. The addition is carried out in small portions, while the suspension for 10...15 minutes reacts, swells and settles to the bottom. If you add too much - then the suspension dissolves, which is undesirable. After the filtered mass is formed at the bottom, the liquid is filtered, the residue is rinsed with a small amount of benzene. Organic phases are combined, washed once with cold water, then acetic acid is added when stirring drop-by-drop (vinegar 70% is suitable). In this case, the remains of borohydride disintegrate with gas release noticeable to the eye. Borane, a poisonous gas, is released, be careful. The addition of acetic acid is completed, when the gas release stops, the mixture is stirred for another 30 minutes, and the product begins to be released.

The yield of this stage - about 75%.

View attachment 607
PRECIPITATION OF EPHEDRINE HYDROCHLORIDE.

The allocation is standard: acid-base extraction, salt planting, washing - and here it is, crystalline powder. A weak aqueous solution of hydrochloric acid in a volume of about a quarter of the volume of benzene is thoroughly mixed with a cooled benzene solution from the previous stage. If after stirring, the solution has not become slightly acidic, then add more acids and mix again. At the same time, the volume of the benzene layer decreases, and the volume of the water layer increases: this ephedrine passes into salt and goes into water. The water layer is separated (it is from below), the benzene is washed two more times with slightly acidic water in portions of a quarter of the volume of benzene. Benzene is thrown out, the aqueous fractions are combined, washed once with a small amount of benzene (the benzene layer will be on top) and once with a portion of dichloromethane (the dichloromethane layer will be from below) 20...30 ml. Solvents are thrown out, the aqueous solution, which has become lighter, is left.

After washing with solvents, ephedrine hydrochloride is added in small portions to the alkalis in dry form and dissolved during cooling (exotherm). At the same time, the color lightens, the mixture becomes cloudy, and with a sufficiently alkaline reaction (pH>11), ephedrine is separated - the base in the form of yellow oil and suspension. The base of ephedrine is extracted in three portions of dichloromethane (the first - 50 ml, the second and third - 20 ml each), with the formation of an emulsion at the border of the layers, it is broken by passing through the filter. The aqueous layer is thrown out, organic extracts are combined, washed once with a weak solution of table salt and once with water, dichloromethane is distilled, preferably with reduced pressure. The residue is dissolved in 50 ml of isopropyl alcohol (IPA), the kobla is rinsed with 20 ml of IPA, alcohol solutions are combined. Drop-by-drop and stirring, concentrated hydrochloric acid (at least 35%) is added until a barely noticeable acidic reaction is achieved. The color of the solution does not change significantly, remaining yellow.

Alcohol is evaporated in a water bath, the remaining thick viscous mass is diluted with a new portion of IPA 20...40 ml, dissolved and evaporated to dry. At the end of the procedure, the product is tried to crystallize, evenly distributed over the evaporation bowl, cooling and supplying a stream of fresh air. It crystallizes without problems, forming a noticeably lightened crust of almost white or light beige color. After crystallization, the bowl with the contents is heated in a water bath for 30 minutes to remove the remnants of moisture, then cooled, the resulting mass is separated with a blade and crushed, preparing for washing.

Pre-prepared acetone is cooled to the lowest possible temperature, and with a small amount grind the resulting product in a mortar. Acetone is filtered. As a rule, this produces a perfectly white powder, which is rinsed directly in the filter with a small amount of acetone, acetone is filtered, the resulting product is dried in a water bath for at least an hour, in the process of drying grinding lumps (while there is a characteristic "creaking").

The yield of this stage is about 80%.

View attachment 608

HIGGS BOSSONSorry if this is a repeated message. What is a reverse refrigerator in this procedure? I’ve never heard of this

 

[plancklong]

Sorry if this is a repeated message. What is a reverse refrigerator in this procedure? I’ve never heard of this

SonnettalesI believe that something got lost in translation! Try replacing the words "reverse refrigerator" with "pressure-equalizing addition funnel", and see what you think then ! There are a few other places in there I'm still working on!

 

[Sonnettales]

I believe that something got lost in translation! Try replacing the words "reverse refrigerator" with "pressure-equalizing addition funnel", and see what you think then ! There are a few other places in there I'm still working on!

plancklongI see! Thank you!

 

[HIGGS BOSSON]

There are inaccuracies in this method.
We are preparing a video on this topic, expect it soon.

 

[None]

There are inaccuracies in this method.
We are preparing a video on this topic, expect it soon.

HIGGS BOSSONHello, was the video made?

 

[lalalander]

But how profitable is it to produce ephedrine with this method? Can we completely rely on this method for production?

 

[Mr.blank00]

hello, everyone. Can someone provide a link for making ephedrine, pseudoephedrine from d-l alananine, metylananine, yesterday someone posted it but I can't find it, please help.

 

[ilovelamp]

hello, everyone. Can someone provide a link for making ephedrine, pseudoephedrine from d-l alananine, metylananine, yesterday someone posted it but I can't find it, please help.

Mr.blank00Uncle Fester has a chapter titled "Cooking Your Own Ephedrine" in his The Secrets of Methamphetamine Manufacture 8th ed. I have been curious about this method for some time now. This could revolutionize clandestine chemistry if its as easy as it sounds. I cant wait to see a step by step video.

 

[SoldadoDeDrogas]

Uncle Fester has a chapter titled "Cooking Your Own Ephedrine" in his The Secrets of Methamphetamine Manufacture 8th ed. I have been curious about this method for some time now. This could revolutionize clandestine chemistry if its as easy as it sounds. I cant wait to see a step by step video.

ilovelampAfter exhausting my resources trying to obtain pseudo pills, I stumbled across this exact method looking through Festers book and became very hopeful once again. From what I understand, it is more or less an equivalent process to brewing your own booze from scratch. Boiling water, adding sugar (or molasses) and yeast - the secret ingredient this time is Benzaldehyde, which is in bitter almond oil in somewhat high concentrations, (depending on brand) from what I understand. More or less %90 pure? You can find this at the grocery store, etc. in the spice/flavoring section. A little bottle of almond oil will literally say "contains: benzaldehyde". I don't know if the almond oil needs to be refined before being added to the 'yeast mash', granted its purity - I don't see the impurities being able to potentially interfere with the fermenting process. Does anybody know? Has anyone fermented Benzaldehyde and gotten to ephedra by these means? Please let me know.

As soon as I figure it out, if anything, I will share the good news. o7

 

[Frit Buchner]

After exhausting my resources trying to obtain pseudo pills, I stumbled across this exact method looking through Festers book and became very hopeful once again. From what I understand, it is more or less an equivalent process to brewing your own booze from scratch. Boiling water, adding sugar (or molasses) and yeast - the secret ingredient this time is Benzaldehyde, which is in bitter almond oil in somewhat high concentrations, (depending on brand) from what I understand. More or less %90 pure? You can find this at the grocery store, etc. in the spice/flavoring section. A little bottle of almond oil will literally say "contains: benzaldehyde". I don't know if the almond oil needs to be refined before being added to the 'yeast mash', granted its purity - I don't see the impurities being able to potentially interfere with the fermenting process. Does anybody know? Has anyone fermented Benzaldehyde and gotten to ephedra by these means? Please let me know.

As soon as I figure it out, if anything, I will share the good news. o7

SoldadoDeDrogasI don't think BAE is 90% benzaldehyde. I think it's 90% ethanol. It would definitely need distilling and you would lose your ass on the price. There's cheaper stuff to get benzaldehyde from. I'm sure butter almond extract could not substitute for benzaldehyde without purification and concentration. I researched it deeply and decided it wasn't a good choice for me. A 55gallon drum can produce 20g of L-pac every 4 days. There's a lot of work to getting that 20g out of 50+ gallons of sludge.

 

[SoldadoDeDrogas]

I don't think BAE is 90% benzaldehyde. I think it's 90% ethanol. It would definitely need distilling and you would lose your ass on the price. There's cheaper stuff to get benzaldehyde from. I'm sure butter almond extract could not substitute for benzaldehyde without purification and concentration. I researched it deeply and decided it wasn't a good choice for me. A 55gallon drum can produce 20g of L-pac every 4 days. There's a lot of work to getting that 20g out of 50+ gallons of sludge.

Frit BuchnerI mean, lemme take a better look, I'm more or less going off Fester's SOMM#8. You are probably correct, if it did ever work, it was probably 20 years ago, after some processing. He makes it sound like it's the answer to all our prayers if ephedra is off limits and there aren't other options. I ought to apply the same skepticism towards some of these things - such as being able to do something in a pinch with the Levo from the inhalers. I should know better by now, that if it was that easy, more if not all would be doing it, and it would be HOT to boot. I am learning quite a bit though putting in the footwork figuring these things out.. the hard way.

 

[Frit Buchner]

I mean, lemme take a better look, I'm more or less going off Fester's SOMM#8. You are probably correct, if it did ever work, it was probably 20 years ago, after some processing. He makes it sound like it's the answer to all our prayers if ephedra is off limits and there aren't other options. I ought to apply the same skepticism towards some of these things - such as being able to do something in a pinch with the Levo from the inhalers. I should know better by now, that if it was that easy, more if not all would be doing it, and it would be HOT to boot. I am learning quite a bit though putting in the footwork figuring these things out.. the hard way.

SoldadoDeDrogasIt works it's been done and done and done. The whole " extracting 20 grams of L-pac from 50 gallons of liquid" Ive seen massive clandestine centrifuges, instead of 15 ml centrifuge tubes, 5 gallon buckets with lids. Or a continuous process slinger. You can buy the for $10s of thousands of dollars, so now you are contemplating a 3 phase 2hp motor, a welded carousel, and at least a basement or garage. You can't just precipitate 50 gallons of solvent because the base is going to cost so much at that amount. Google scholar will show you 100's of write ups on it. I think I could make phenyl acetate cheaper. Once I read a reaction on Science madness. The guy needed anhydrous ethanol. He broke ethyl acetate to get it and I thought that was insane when you could distill it yourself, but you know, he had anhydrous ethanol in less than 1 hour and ethyl acetate is $25/liter so if you only need 150ml. It. Looks. A. Lot. More attractive

 

[SoldadoDeDrogas]

It works it's been done and done and done. The whole " extracting 20 grams of L-pac from 50 gallons of liquid" Ive seen massive clandestine centrifuges, instead of 15 ml centrifuge tubes, 5 gallon buckets with lids. Or a continuous process slinger. You can buy the for $10s of thousands of dollars, so now you are contemplating a 3 phase 2hp motor, a welded carousel, and at least a basement or garage. You can't just precipitate 50 gallons of solvent because the base is going to cost so much at that amount. Google scholar will show you 100's of write ups on it. I think I could make phenyl acetate cheaper. Once I read a reaction on Science madness. The guy needed anhydrous ethanol. He broke ethyl acetate to get it and I thought that was insane when you could distill it yourself, but you know, he had anhydrous ethanol in less than 1 hour and ethyl acetate is $25/liter so if you only need 150ml. It. Looks. A. Lot. More attractive

Frit BuchnerThere is a NileRed video on YT in which he obtains a relatively pure sample of 'essential oil of almond' or something from ebay and says it is pure enough to be used -as is- in reactions, but goes on to purify it anyway. Fester says to run a vacuum for a few minutes to remove the HCN. It is mentioned BAE/benzaldehyde is controlled substance in USA which is funny because I literally grabbed a small bottle of BAE at the market yesterday listing as the only ingredient: benzaldehyde. I realize that this does sound better on paper.

I'm sorry, my friend, Frit, I'm not able to make much sense of what you are saying. What you've seen and decided was or wasn't practical for you or whomever else isn't necessarily going to be true for everyone. I'm trying to set up production, brother, if you know what I mean, and what's stopping me, as of now, is lack of a certain ingredient. For now I've got Ma Huang as a last resort , but I'm not even trying to go that route if I don't have to. My main priority at the moment, and going forward, is not draw any attention or leave a trail whatsoever.

If one wanted to step up production, Fester says, this is a viable alternative from buying pills or extracting plants. If one wanted to start a 5Gal bucket or two for fermenting benzaldhyde, contiuously, none of the equipment you speak of is necessary, and the cost of molasses/sugar/yeast/BAE isn't relevant to me. Though a distillation/reflux apparatus, etc. would be nice and helpful, I'm not there yet.

Extracting the L-PAC is relatively simple, (according to this outline in somm). Filter the mash and use a toluene or ether wash to pull it and evap. I'm trying to see this process through to ephedra, and so the next step is to use methylamine for reduction. If that has been done and done, then noone is really talking about it or seems to know much, that I am able to find. Forgive me for seeking elaboration and taking everything with a grain of salt, in spite of all the flexing and street cred. As I said, I am learning a great deal in the process of sorting it all out, in any event. Thank you for your time and input. o7

 

[Frit Buchner]

None of the administration nor anyone else has responded to me pointing out that the pictures of the chemicals at the end represent ephedrine nor ephedrine or pseudoephedrine. I am also intrigued at what mechanism turned this a chiral molecule into some other with specific stereo arrangement of 2 chiral carbons. Usually that takes a chiral reactant or produces a racemic product. Please, I must know this witchcraft

 

[Frit Buchner]

Here's what I come up with, constituents of butter almond extract, Water, Alcohol (36%) and oil of bitter almonds.
State and federal law say that almond extract must contain at least 1% bitter almond oil . So water, more than 36% since it is listed first, 36% ethanol, that's at least 73% of it