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GhostChemist

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The synthesis of Ephedrine hydrochloride is proceeding according to Scheme 1.
LklAtFKE9r

Scheme 1

Were've carried out 3 synthesis of Ephedrine with 1, 1.5 and 2 equivalents of NaBH4 to methcathinone

Starting reagents and materials for a one synthesis:


  • 10 g of purified methcathinone hydrochloride
  • 40-50 mL of 88% ethanol
  • 2 g (1 equivalent (Eq)), 2.95 g (1.5 Eq) and 3.7 g (2 Eq) of sodium borohydride
  • 300 mL of distilled water
  • 250-300 + 20 mL of Dichloromethane (DCM)
  • 15 mL of 14% hydrochloric acid
  • 10-15 mL of ethyl acetate
  • 10 mL of cold acetone (temperature not exceeding -5°C)
  • Magnetic stirrer with heating
  • 1 L three-necked flask
  • Beakers
  • Separatory funnel
  • Reflux Condenser
  • Thermometer
  • Glass corks
  • pH indicator paper.

Download Video

The starting components are presented in Figure 1.
Gm6DV2keTt

Fig 1

Methcathinone hydrochloride is placed into the flask, and ethanol is added until dissolved. Figure 2
7dV2Ywi3yK

Fig 2

After complete dissolved of methcathinone, sodium borohydride is added in very small portions. The reaction mixture temperature should be in the range of 20-30°C. Figure 3
CVI9exBSE3

Fig 3

After the addition of the entire amount of sodium borohydride, the reaction mixture is stirred for 24 hours. Figure 4
VI6uSH3CbU

Fig 4

After 24 hours, 200 mL of water is added to the reaction mixture until most of the precipitate dissolves. Figure 5
WPoKaSDdHG

Fig 5

After the addition of water, the mixture is stirred for approximately 20-30 minutes. Figure 6
Gtj5rxqH8B

Fig 6

To the obtained solution, 50 mL of DCM were added. Figure 7
UHIFRurik3

Fig 7

The mixture with added DCM was stirred for 5-10 minutes. Figure 8
DBXic5LQRJ

Fig 8

The obtained mixture is transferred in portions of 50-100 mL into a separatory funnel and extracted with additional portions of DCM. The total volume of DCM for extraction is 250-300 mL. Figure 9
TTJX1x8Q6R

Fig 9

The obtained ephedrine extract in DCM is transferred to a flask, and 50 mL of water is added. The extract in DCM should have an alkaline pH. Figure 10
87PAd5fYmG

Fig 10

To the reaction mixture, 14% hydrochloric acid (12-17 mL in experiment 1.5 eq and for Met-reduction) is added dropwise until a consistently slightly acidic pH was obtained. Figure 11
MeUjYo023N

Fig 11

After the addition of the hydrochloric acid solution and reaching a stable slightly acidic pH, the reaction mixture was stirred for 30-40 minutes. Figure 12
JjdHpvZ9gS

Fig 12

After stirring the mixture for 30-40 minutes, the mixture is allowed to separate. Figure 13
5XUBvPgkqZ

Fig 13

The layer of DCM was separated and again added 50 mL of water to extract the ephedrine hydrochloride. If the solution has an alkaline or neutral pH, a small portion of hydrochloric acid is added. The pH should be slightly acidic. Figure 14
CmFM0wnILj

Fig 14

The aqueous layers with an acidic pH are combined, and 20 mL of DCM was added to them for purification from organic impurities. Figure 15
FEG2K835Mq

Fig 15

The mixture is shaken and left for layer separation in a separatory funnel. Figure 16
TKIj9D7C5m

Fig 16

The layer of DCM was discarded. The aqueous layer was filtered through a paper filter. Figure 17
3LX1mW0OP9

Fig 17

The filtered solution was evaporated at a temperature of 100-130°C. Figure 18
DsKlIYpmMq

Fig 18

Evaporation continues until crystallization occurs. Figure 19
MRF8V4y0Of

Fig 19

To confirm the identity of the Ephedrine, a qualitative test was conducted. A few ml of CuSO4 solution, a few drops of NaOH solution, and 2-3 mL of ethyl acetate are added to the aqueous solution of the crystal. Ephedrine produces a pink coloration in the ethereal layer (Test Tube 2). In comparison, methcathinone does not show such a reaction (Test Tube 1). Additionally, when the obtained product is heated with a solution of K3[Fe(CN)6] and alkali, it produces the smell of benzaldehyde, that is indicating the presence of ephedrine. Ephedrine hydrochloride crystals have a bitter taste. Figure 20
SjI78LQbz0

Fig 20

The crystals are transferred to a filter and treated with a mixture of 15 mL of ethyl acetate and 10 mL of cold acetone (not exceeding -5°C). The mixture is quickly and thoroughly stirred. The crystals are allowed to settle for 20-30 seconds and then vacuum-filtered. The washed crystals are air-dried. Figure 21
Cnhxf6T4yL

Fig 21

The yield of ephedrine hydrochloride is 6.1-7.6 g or 60 - 75%



Analysis

Reagents and materials
  • Ephedrine hydrochloride synthesis by 1.5 Eq; 2 Eq and 1 Eq NaBH4
  • Simon`s reagent (2% water solution of Na2CO3; 1% water solution of sodium nitroprusside Na2[Fe(CN)5NO]*2H2O; solution of acetaldehyde in ethanol)
  • Reagent for Chen-Kao reaction (1% water solution of acetic acid; 1% water solution of CuSO4*5H2O; 2N water solution of NaOH)
  • Reagent Ninhydrin (10% solution of Ninhydrin in ethanol)
  • NaOH
  • Ethyl acetate
  • Ethanol 88%
  • TLC Silica gel
  • UV-lamp
  • Glass Pasteur pipettes
  • Refractometer
  • Watch glasses
  • Measuring flask 100 ml 20 ℃ (B)
  • Distilled water

3 samples of Ephedrine hydrochloride synthesis by 1.5 Eq; 2 Eq and 1 Eq NaBH4 were obtained. Fig 22
JASulXsvcL

Fig 22

All obtained samples of Ephedrine hydrochloride were tested with the qualitative Simon's reaction. All ephedrine samples showed a negative reaction for the presence of meth. As a comparison, a control determination was carried out. Metcat also did not exhibit a qualitative Simon's reaction; it is possible that it is not specific to katinons. Fig 23
W23EbsjIqr

Fig 23

Subsequently, the Chen's reaction was conducted. All samples of Ephedrine hydrochloride and sample of Methcathinone exhibited a positive reactions. Fig 24
XRw4U9YLF6

Fig 24

The obtained samples of Ephedrine hydrochloride were tested using thin-layer chromatography with visualization under a UV lamp. Prepared aqueous solutions of Ephedrine hydrochloride were applied to the plate and dried. Fig 25
4k8YgDqb6e

Fig 25

Subsequently, the plate was placed in a mixture of solvents (50 mL of 88% ethanol, 25 mL of water, 5 mL of ethyl acetate, and 20 mL of 0.5% NaOH solution). Fig 26
JJirBZGeSv

Fig 26

Under UV irradiation, only marks of the main substance are visible. Fig 27
WoZk5lVORr

Fig 27

The second chromatogram was obtained in a solvent mixture of 70 mL of 88% ethanol and 10 mL of ethyl acetate. Fig 28
GPt6CahuKz

Fig 28

Visualization under the UV lamp revealed the presence of a single component and a very small amount of impurities. Fig 29
H3D6XPzlYs

Fig 29

Next, the plate was sprayed with a ninhydrin solution. Fig 30
NLEMBub4Gx

Fig 30

The plate was dried, and visualization was carried out by heating the plate to 120°C. Fig 31
V6fok1thuD

Fig 31

Considering the very close chemical relationship between Methcathinone and Ephedrine, achieving a clear separation on the chromatogram is quite challenging. The most reliable method is measuring the refractive index of aqueous solutions of Ephedrine prepared with precisely defined concentrations. For this purpose, solutions were prepared with concentrations: 1st sample - 1.5 Eq 1% (1 g in 100 mL), 2nd - 2 Eq 5% (5 g in 100 mL), 3rd - 1 Eq 8% (8 g in 100 mL). Fig 32
VFTjsPZcfi

Fig 32

Refractive index values for solutions of Ephedrine hydrochloride with precisely defined concentrations are provided in Table 1.

Table 1. Concentrations of Ephedrine hydrochloride solutions and refractive index

Refractive index
nD20
Concentrations of Ephedrine hydrochloride, %
1.334
0.5
1.335
1
1.336
1.5
1.337
2
1.338
2.5
1.339
3
1.340
3.5
1.341
4
1.342
4.5
1.343
5
1.344
5.5
1.345
6
1.346
6.5
1.347
7.5
1.348
8
1.349
8.5
1.350
9
1.351
9.5
1.352
10
1.353
10.5

For the 1.5 Eq solution with a concentration of 1%, the refractive index was 1.3349. Fig 33
5lSZnaBcgo

Fig 33

For the 2 Eq solution with a concentration of 5%, the refractive index was 1.3429. Fig 34
Vms35cCqBH

Fig 34

For the 1 Eq solution with a concentration of 8%, the refractive index was 1.3493. Fig 35
KnQpaBRsjZ

Fig 35

Based on the obtained data, the use of 1 equivalent of sodium borohydride leads to the presence of impurities in the sample after synthesis. Subsequently, it is necessary to use no less than 1.5 equivalents of borohydride for the complete reduction of Methcathinone to Ephedrine. The Raman spectroscopy spectrum of the racemic Ephedrine hydrochloride sample is presented in Fig 36.
HN2l1npsho

Fig 36
 
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bigbadbear

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Thank you for your continuous effort and perseverance👌👌👍
 

Mo0odi

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I loved all of your synthesis and reports with pictures

Really thank you for all your efforts


I hope and hope that you will record a video of your amazing work


Thank you 🌷
 

Wiscounsin

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Thank you, that is love for chemistry. Holy God. I'm paralyzed between Mr. Patton and Mr. Chemical Ghost, two experts. I kneel at his feet. Really thank you for sharing your knowledge.
 

OrgUnikum

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By what magic does the reduction of racemic methcathione produce (-)-ephedrine as claimed? And If one does not get either (-)-ephedrine or (+)-pseudoephedrine whats it good for? The mixture of all possible stereoisomeres is not a good drug but its use is highly discouraged as its very unhealthy. Really bad. The further reduction will produce racemic methamphetamine whats far easier made from MeNH2 and P2P.

Be warned! This is not the Ephedrine you are after, this will not make Crystal Meth on reduction!

GhostChemist, I really like most of your contributions but this now is very misleading, it is as presented also obviously factually wrong and I do not know why you do this, as in the long run in clandestine chemistry its only reputation what counts and you are doing yourself no favor here, trust me.
 
View previous replies…

Wiscounsin

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By what magic does the reduction of racemic methcathione produce (-)-ephedrine as claimed? And If one does not get either (-)-ephedrine or (+)-pseudoephedrine whats it good for? The mixture of all possible stereoisomeres is not a good drug but its use is highly discouraged as its very unhealthy. Really bad. The further reduction will produce racemic methamphetamine whats far easier made from MeNH2 and P2P.

Be warned! This is not the Ephedrine you are after, this will not make Crystal Meth on reduction!

GhostChemist, I really like most of your contributions but this now is very misleading, it is as presented also obviously factually wrong and I do not know why you do this, as in the long run in clandestine chemistry its only reputation what counts and you are doing yourself no favor here, trust me.
OrgUnikumSorry to bother you. I was a little surprised by what you wrote. I thank you for your advice on ephedrine, but who told you that I want to reduce the result of this synthesis. I think there has been a misunderstanding. I have only commented that these two experts from the forum that I have named do a great job sharing their knowledge and guiding people. On the other hand, I have no idea about chemistry. I wish I met them in person to learn from them on a daily basis. Just that without more. I do not produce methamphetamine. Greetings mate.
 

btcboss2022

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By what magic does the reduction of racemic methcathione produce (-)-ephedrine as claimed? And If one does not get either (-)-ephedrine or (+)-pseudoephedrine whats it good for? The mixture of all possible stereoisomeres is not a good drug but its use is highly discouraged as its very unhealthy. Really bad. The further reduction will produce racemic methamphetamine whats far easier made from MeNH2 and P2P.

Be warned! This is not the Ephedrine you are after, this will not make Crystal Meth on reduction!

GhostChemist, I really like most of your contributions but this now is very misleading, it is as presented also obviously factually wrong and I do not know why you do this, as in the long run in clandestine chemistry its only reputation what counts and you are doing yourself no favor here, trust me.
OrgUnikumHello, I usually don't comment on other people's comments, to be honest, but this time I couldn't help it.
I have great respect for both of you @OrgUnikum and @GhostChemist , and I am well aware of your mastery of chemistry.
It's true that @GhostChemist was not accurate with that report, as it's clear that it yields a racemic product, even though throughout the entire procedure, he only mentions ephedrine without specifying a particular enantiomer, except in the report, which obviously cannot be the product produced with that process.

Having said that, in my opinion, we shouldn't be so "hard," I mean in the way we express it (possibly the same thing could be said differently), with someone who is sharing their work and knowledge altruistically just to help others.
I think we should appreciate more people like this; that's how I see it, even if they made a mistake in this case.
It's my point of view, which doesn't have to coincide with anyone else's, of course.

On the other hand, carefully examining the process has made me consider the route starting from 4-Methylpropiophenone without going through ephedrine, and I believe it can be done:
4'-Methylpropiophenone -> Ephedrone/Methcathinone -> (R) Ephedrone/Methcathinone -> (R) Secondary amine -> (R) Methamphetamine.
At the moment I will do it from (R) isomer because I think that any of the reductions made it would change like ephedrine does
I'll let you know how it goes because right now, I'm focused on finding a way to racemize Meth. I have a couple of feasible routes; I'm working on it ;-)
 

OrgUnikum

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Hello, I usually don't comment on other people's comments, to be honest, but this time I couldn't help it.
I have great respect for both of you @OrgUnikum and @GhostChemist , and I am well aware of your mastery of chemistry.
It's true that @GhostChemist was not accurate with that report, as it's clear that it yields a racemic product, even though throughout the entire procedure, he only mentions ephedrine without specifying a particular enantiomer, except in the report, which obviously cannot be the product produced with that process.

Having said that, in my opinion, we shouldn't be so "hard," I mean in the way we express it (possibly the same thing could be said differently), with someone who is sharing their work and knowledge altruistically just to help others.
I think we should appreciate more people like this; that's how I see it, even if they made a mistake in this case.
It's my point of view, which doesn't have to coincide with anyone else's, of course.

On the other hand, carefully examining the process has made me consider the route starting from 4-Methylpropiophenone without going through ephedrine, and I believe it can be done:
4'-Methylpropiophenone -> Ephedrone/Methcathinone -> (R) Ephedrone/Methcathinone -> (R) Secondary amine -> (R) Methamphetamine.
At the moment I will do it from (R) isomer because I think that any of the reductions made it would change like ephedrine does
I'll let you know how it goes because right now, I'm focused on finding a way to racemize Meth. I have a couple of feasible routes; I'm working on it ;-)
btcboss2022You are right. Resolving into its stereoisomeres the methcathione (better: use a chiral synth), this should be far easier then doing it with Meth, and then reduce the chiral methcathione all through to the chiral Amine.
IIRC it depends on what you use for the reduction if there is retention or inversion of the product. Pd/C and Pt does rather inverse, most others keep it.
Uups, just remembered, here in this case the chral orientation on the 2- Position where the Amine group sity is always stable as this part is never touched at all.
It is just logical. So no need to worry.

Jans suggested method makes sense, the Topic as posted sadly not so much.

I also did not flame the ass off somebody here, I offered rightful and educated constructive criticism. if somebody cannot cope with this then the Internet is not the place for him, sorry.
 

G.Patton

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By what magic does the reduction of racemic methcathione produce (-)-ephedrine as claimed? And If one does not get either (-)-ephedrine or (+)-pseudoephedrine whats it good for? The mixture of all possible stereoisomeres is not a good drug but its use is highly discouraged as its very unhealthy. Really bad. The further reduction will produce racemic methamphetamine whats far easier made from MeNH2 and P2P.

Be warned! This is not the Ephedrine you are after, this will not make Crystal Meth on reduction!

GhostChemist, I really like most of your contributions but this now is very misleading, it is as presented also obviously factually wrong and I do not know why you do this, as in the long run in clandestine chemistry its only reputation what counts and you are doing yourself no favor here, trust me.
OrgUnikumHello. First of all, this method is developed, described and recorded to provide information to BB Forum for free and it cost a lot of efforts and time. Secondly, there is only Raman's report statement that it's (-)-ephedrine. So far as many chemists know, Raman, especially partitive, cannot determine stereoisomers precisely. There are no any statements that the resulting ephedrine is (-)-ephedrine. This method describes racemic ephedrine hydrochloride production from ephedrone.

Be warned! This is not the Ephedrine you are after, this will not make Crystal Meth on reduction!
Please, do not shame yourself. You statement about "not correct" isomer is bullshit. It's known fact that racemic meth is the result of ephedrine reduction. By other words for you, you'll d,l-methamphetamine (isomer mixture) from any ephedrine isomers after reduction by Birch or any other way.

GhostChemist, I really like most of your contributions but this now is very misleading, it is as presented also obviously factually wrong and I do not know why you do this, as in the long run in clandestine chemistry its only reputation what counts and you are doing yourself no favor here, trust me.
I have some ideas why do you criticize by such populist and nonsense comments here, probably you want to get some reputation and use it for your affairs on the Forum. I can tell you, that we'll look after you. Please, If you decided criticize, do it in accordance with facts.
 
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NAGAINAGAYOSHI

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Hello. First of all, this method is developed, described and recorded to provide information to BB Forum for free and it cost a lot of efforts and time. Secondly, there is only Raman's report statement that it's (-)-ephedrine. So far as many chemists know, Raman, especially partitive, cannot determine stereoisomers precisely. There are no any statements that the resulting ephedrine is (-)-ephedrine. This method describes racemic ephedrine hydrochloride production from ephedrone.


Please, do not shame yourself. You statement about "not correct" isomer is bullshit. It's known fact that racemic meth is the result of ephedrine reduction. By other words for you, you'll d,l-methamphetamine (isomer mixture) from any ephedrine isomers after reduction by Birch or any other way.


I have some ideas why do you criticize by such populist and nonsense comments here, probably you want to get some reputation and use it for your affairs on the Forum. I can tell you, that we'll look after you. Please, If you decided criticize, do it in accordance with facts.
G.PattonIsnt a known fact that ephedrine reduces to dmeth? Whole p2p does racemic
 

NAGAINAGAYOSHI

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OrgUnikum

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What else would you want to do with it? You cannot use it as drug as it is dangerous to the health, the mixture of natural and unnatural Stereoisomeres is regarded is as bnad as it gets as the compounds counteract and elevate each other, its described in the MERCK Index for example.
 

Wiscounsin

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What else would you want to do with it? You cannot use it as drug as it is dangerous to the health, the mixture of natural and unnatural Stereoisomeres is regarded is as bnad as it gets as the compounds counteract and elevate each other, its described in the MERCK Index for example.
OrgUnikumOK THANKSSSSS BROTHERRRRRR
 

btcboss2022

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What else would you want to do with it? You cannot use it as drug as it is dangerous to the health, the mixture of natural and unnatural Stereoisomeres is regarded is as bnad as it gets as the compounds counteract and elevate each other, its described in the MERCK Index for example.
OrgUnikumAnyway isomer resolution could be done over the methcathinone with tartaric acid and fix the racemic ephedrine in that case would separate the (S)Methcathinone to have (S)ephedrine to reduce to (R)Methamphetamine
 
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