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Alprazolam (Xanax) synthesis. Small scale.

G.Patton

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Introduction

I would love to represent you this simple method of Xanax (Alprazolam; Xanor, Niravam; 8-chloro-1-methyl-6-phenyl-4H-benzo[f][1,2,4]triazolo[4,3-a][1,4]diazepine) synthesis. It doesn't take elaborated glassware or exotic reagents, all used techniques are extremely simple. Nevertheless, chemist have to pay attention to safety and use PPE.

Equipment and glassware:

Reagents:

  • 2-Amino-5-chloro benzophenone 0.232 g, 1 mmol;
  • Chloroacetyl chloride 1.2 mL, 2 mmol;
  • Ammonium acetate (NH4OAc) 0.23 g, 3 mmol;
  • Potassium carbonate (K2CO3) 0.97 g, 7 mmol;
  • Distilled water, 1 L;
  • Potassium hydroxide (KOH) 0.22 g, 4 mmol;
  • Acetic anhydride 0.18 mL, 2 mmol;
  • Hydrazine hydrate (N2H5OH) 4 mmol, 0.2 mL
  • Acetic acid AcOH 25 ml;
  • Ethanole (EtOH) 100 ml 95%.
HmUNfQIuqd

Boiling Point: 509.0±60.0 °C at 760 mm Hg;
Melting Point: 228-228.5 °C;
Molecular Weight: 308.765 g/mol;
Density: 1.4±0.1 g/ml (20 °C);
CAS Number: 28981-97-7.

Procedures

Synthesis of 7-chloro-5-phenyl-1H benzo[e][1,4]diazepin-2(3H)-one (nordiazepam) (1)
To a vigorously stirred of 2-amino-5-chloro benzophenone (0.232 g, 1 mmol) in a pear-shaped flask (10-50 ml), chloroacetyl chloride (1.2 mL, 2 mmol) was added drop wise at room temperature under solvent-free conditions during 30 min and the progress of reaction was monitored by TLC. After completion of the reaction, NH4OAc (0.23 g, 3 mmol) and K2CO3 (0.42 g, 3 mmol) were added to the mixture at room temperature under solvent-free conditions and stirred for 2.5 h. When the reaction was completed, as it was shown by TLC, the water (30 mL) was added and the product was filtered off via paper filter, washed with more distilled water (2 x 100 mL) and dried in vacuum desiccator. The product was obtained in high yield and purity (94% yield) and was used in the next step without any purification. m.p. = 212–214 °C.
M43Nt1JgAC
Synthesis of 1-acetyl-7-chloro-5-phenyl-1H-benzo[e][1,4]-diazepin-2(3H)-one (2)
To a vigorously stirred mixture of nordiazepam (1) (0.27 g, 1 mmol) in a pear-shaped flask (10-50 ml), a powder mixture of K2CO3 (0.55 g, 4 mmol)/KOH (0.22 g, 4 mmol) and acetic anhydride (0.18 mL, 2 mmol) was added. The progress of the reaction was monitored by TLC. After completion of the reaction (3 h), water (3 x 10 mL) was added and the 1-acetyl-7-chloro-5-phenyl-1H-benzo[e][1,4]diazepin-2(3H)-one (2) was easily isolated by a simple filtration in more than 80% yield with high purity. The product was used in the next step without any purification. m.p. = 163–165 °C.
EAgay4c7u2
Synthesis of 8-chloro-1-methyl-6-phenyl-4H-benzo[f][1,2,4]triazolo[4,3-a][1,4]diazepine (Alprazolam, Xanax) (3)
A solution of 1 mmol (0.31 g) of 1-acetyl-7-chloro-5-phenyl-1H-benzo[e][1,4]diazepin-2(3H)-one (2), hydrazine hydrate N2H5OH (4 mmol, 0.2 mL) and NaOAc (4 mmol, 0.2 mL) in 25 ml of AcOH was refluxed for 12 h in a pear-shaped flask (100 ml) with a reflux condenser. The progress of the reaction was monitored by TLC. After completion of the reaction, the solution was cooled and the product was filtered, washed with water, dried, and crystallized from EtOH. (75% yield); m.p. = 228–230 °C.
Lhpr1EMvkd
 
Last edited:

Jack

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G.Patton are you aware that in the pictures you provide you depict acetic anhydride as diethyl ether?
 

G.Patton

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G.Patton are you aware that in the pictures you provide you depict acetic anhydride as diethyl ether?
JackSorry, I forgot about oxygen %)
 

Hedgie

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Have you run this experiment successfully yourself? I am actually very interested in this particular synthesis; I recognize it from a paper that I just read recently and I was really pleasantly surprised by its simplicity. I just want to know if you have had success with this route because I have been seriously considering giving it a try myself. Please let me know if you have tried this in your lab and how it worked out??
 

G.Patton

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Have you run this experiment successfully yourself? I am actually very interested in this particular synthesis; I recognize it from a paper that I just read recently and I was really pleasantly surprised by its simplicity. I just want to know if you have had success with this route because I have been seriously considering giving it a try myself. Please let me know if you have tried this in your lab and how it worked out??
HedgieI've never tried this synthesis, but it's quite simple method and doesn't take an expensive glassware or reagents. If you need my assistant, I can help you. Ask me in private message.
 
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nbnbbnryrtyrt

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Is there any simple way to synthesize 2-Amino-5-chloro benzophenone or is it sold anywhere?
 

beetlebb

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Have you run this experiment successfully yourself? I am actually very interested in this particular synthesis; I recognize it from a paper that I just read recently and I was really pleasantly surprised by its simplicity. I just want to know if you have had success with this route because I have been seriously considering giving it a try myself. Please let me know if you have tried this in your lab and how it worked out??
Hedgie
Hey Hedgie,
do you have the lit, information. I would like to read it. I find this syn very interesting
 

G.Patton

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Last edited by a moderator:

beetlebb

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Got it Patton, just read the Nitrazepam link. attached below the reference too.
 

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SoraQ

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Thank you Patton for your impressive work, I want to ask you after i make a raw alprazolam, How do i put it in pills? What element is placed with alprazolam/Amphetamine etc.. to have a solid pills?


p.s your brain is really a storage of data, lol i don't know how you have that much of information.
 

G.Patton

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Thank you Patton for your impressive work, I want to ask you after i make a raw alprazolam, How do i put it in pills? What element is placed with alprazolam/Amphetamine etc.. to have a solid pills?


p.s your brain is really a storage of data, lol i don't know how you have that much of information.
SoraQThanks for kind words, see Tableting
 

madmoney69

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anyone working on this?
 

KokosDreams

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Agilent1100DAD

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I'd be interested in hearing about a report too
KokosDreamsJust waiting on the chloroacetyl chloride to arrive and I’ll have everything I need. I’ll write up a little report about it, I’m looking to scale this up by x100, so I’ll also be playing around with that after the small scale synth. I have access to a copious amount of 2-Amino-5-chloro benzophenone and am willing to share , as well as perhaps make a video on this synthesis.

I believe this is a very important one for people to learn, perhaps since alprozolam is so cheap to make, this would lead to less fentanyl laced Xanax bars. Only one can hope. It’s important to note that the main precursor, 2-Amino-5-chloro benzophenone, is NOT a scheduled precursor!!
@madmoney69
@Hedgie
 

Field7

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Just waiting on the chloroacetyl chloride to arrive and I’ll have everything I need. I’ll write up a little report about it, I’m looking to scale this up by x100, so I’ll also be playing around with that after the small scale synth. I have access to a copious amount of 2-Amino-5-chloro benzophenone and am willing to share , as well as perhaps make a video on this synthesis.

I believe this is a very important one for people to learn, perhaps since alprozolam is so cheap to make, this would lead to less fentanyl laced Xanax bars. Only one can hope. It’s important to note that the main precursor, 2-Amino-5-chloro benzophenone, is NOT a scheduled precursor!!
@madmoney69
@Hedgie
Agilent1100DADThere's "scheduled" and then there's "watched". Long, long list of watched chemicals. Even acetone and 40% Hydrogen Peroxide are watched (depending on part the volume of the purchase). Just about anything anhydrous is watched. "Why does so and so need 4 liters of anhydrous hydrazine shipped to their *apartment?" They're not baking cookies; that's for sure...
 

Yiazo

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how many grams of alprazolam powder can be obtained with this formula ?
 

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Last edited:

Agilent1100DAD

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Hey guys; I’ve done a similar synthesis and I’ve successfully produced about 50 g of diazepam. That was a while ago but now have enough precursor and solvents to produce about 80 g of alprazolam.

2-Amino-5-chloro benzophenone is readily available on sigma aldrich. It’s dirt cheap. I’ll post some photos of my diazepam synthesis.

Im new to this forum but have a lot of experience in general synthesis, analytical chemistry and drug delivery system development. My last company had a DEA schedule I & 3 research and manufacturing license, so I believe I have some knowledge I would like to share with the members here in due time. The following photos are from the diazepam synthesis. That was my first time doing it so the yield was low (60%) and the purity was sub-standard (95%) before re-crystallization. Purity was confirmed via LC-MS and structure confirmed via ATR-FTIR
 

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jarredreyes0303

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Hey guys; I’ve done a similar synthesis and I’ve successfully produced about 50 g of diazepam. That was a while ago but now have enough precursor and solvents to produce about 80 g of alprazolam.

2-Amino-5-chloro benzophenone is readily available on sigma aldrich. It’s dirt cheap. I’ll post some photos of my diazepam synthesis.

Im new to this forum but have a lot of experience in general synthesis, analytical chemistry and drug delivery system development. My last company had a DEA schedule I & 3 research and manufacturing license, so I believe I have some knowledge I would like to share with the members here in due time. The following photos are from the diazepam synthesis. That was my first time doing it so the yield was low (60%) and the purity was sub-standard (95%) before re-crystallization. Purity was confirmed via LC-MS and structure confirmed via ATR-FTIR
hello1321sheesh brother thats some fancy looking equipment ! you just do this as a hobby ? would love to be friends, i grow mushrooms and weed maybe we can share products and chat it up. feel free to message me
 

G.Patton

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Hey guys; I’ve done a similar synthesis and I’ve successfully produced about 50 g of diazepam. That was a while ago but now have enough precursor and solvents to produce about 80 g of alprazolam.

2-Amino-5-chloro benzophenone is readily available on sigma aldrich. It’s dirt cheap. I’ll post some photos of my diazepam synthesis.

Im new to this forum but have a lot of experience in general synthesis, analytical chemistry and drug delivery system development. My last company had a DEA schedule I & 3 research and manufacturing license, so I believe I have some knowledge I would like to share with the members here in due time. The following photos are from the diazepam synthesis. That was my first time doing it so the yield was low (60%) and the purity was sub-standard (95%) before re-crystallization. Purity was confirmed via LC-MS and structure confirmed via ATR-FTIR
hello1321You can sell them via BB market, if you want. Also, can get Manufacturer status. Don't hesitate to write me in PM, I'll help you.
@jarredreyes0303 You also very welcome!
 

G.Patton

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yea was talking with someone about opening a vendor shop , do you sell your results or would you send sample to give feedback ?
jarredreyes0303>>>do you sell your results or would you send sample to give feedback ?
What do you mean? Which results? I suggest to sell your product in BB marketplace.
 

inguhyawetrust

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Hey guys; I’ve done a similar synthesis and I’ve successfully produced about 50 g of diazepam. That was a while ago but now have enough precursor and solvents to produce about 80 g of alprazolam.

2-Amino-5-chloro benzophenone is readily available on sigma aldrich. It’s dirt cheap. I’ll post some photos of my diazepam synthesis.

Im new to this forum but have a lot of experience in general synthesis, analytical chemistry and drug delivery system development. My last company had a DEA schedule I & 3 research and manufacturing license, so I believe I have some knowledge I would like to share with the members here in due time. The following photos are from the diazepam synthesis. That was my first time doing it so the yield was low (60%) and the purity was sub-standard (95%) before re-crystallization. Purity was confirmed via LC-MS and structure confirmed via ATR-FTIR
Agilent1100DAD@Agilent1100DAD how can someone send you a PM?
 
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