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Alprazolam (Xanax) synthesis. Small scale.

nbnbbnryrtyrt

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

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...
 

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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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?
 

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.
 

shadowsoflite

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Hydrazine, seriously? You realize how dangerous that is right? Just saying, maybe a warning to everyone would be helpful
 

Agilent1100DAD

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Alright, I did the first part of the alprazolam synthesis, which involved a “solvent free” procedure. I dropped chloroacetyl chloride into the benzophenone compound over the course of 30 minutes. I then added potassium carbonate and ammonium acetate and let it stir for 2.5 hours. I filtered and washed with water. I got about 75% yield of nordiazepam. Confirmed with MP and TLC.

I will now convert the nordiazepam (after a taste test ;)) into 1-acetyl-7-chloro-1H-benzo 1,4 diazepin. Then convert that into alprazolam, using hydrazine mono hydrate. I will be doing this step outside lol.

I’m going to redo this step but I’m going to scale up x10. I’ll post photos.

UkF8JTreqX
 
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jarredreyes0303

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Alright, I did the first part of the alprazolam synthesis, which involved a “solvent free” procedure. I dropped chloroacetyl chloride into the benzophenone compound over the course of 30 minutes. I then added potassium carbonate and ammonium acetate and let it stir for 2.5 hours. I filtered and washed with water. I got about 75% yield of nordiazepam. Confirmed with MP and TLC.

I will now convert the nordiazepam (after a taste test ;)) into 1-acetyl-7-chloro-1H-benzo 1,4 diazepin. Then convert that into alprazolam, using hydrazine mono hydrate. I will be doing this step outside lol.

I’m going to redo this step but I’m going to scale up x10. I’ll post photos.

hello1321good stuff brother very impressive work !
 

KokosDreams

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Alright, I did the first part of the alprazolam synthesis, which involved a “solvent free” procedure. I dropped chloroacetyl chloride into the benzophenone compound over the course of 30 minutes. I then added potassium carbonate and ammonium acetate and let it stir for 2.5 hours. I filtered and washed with water. I got about 75% yield of nordiazepam. Confirmed with MP and TLC.

I will now convert the nordiazepam (after a taste test ;)) into 1-acetyl-7-chloro-1H-benzo 1,4 diazepin. Then convert that into alprazolam, using hydrazine mono hydrate. I will be doing this step outside lol.

I’m going to redo this step but I’m going to scale up x10. I’ll post photos.

Agilent1100DADHey there :) We've been in touch here in the comment section some months ago.
Your profile is closed for DMs, can you reach out to me? I have some things to discuss!
 

Agilent1100DAD

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Alright guys I redid the first step of the synthesis (nordiazepam synthesis) but scaled up x10. I got about 60% yield this time.

Issues I had which lead to lower yield:

1. during the vacuum filtration step, my fritted filter was letting product through so I had to switch and re filter everything.

2. I added 10 mL of chloroacetyl chloride instead of 12 mL; I was luckily able to add the last 2mL towards the end of the 2.5 hr mark.

*I also will do a triturarion in a flask next time, post vacuum filtration wash; perhaps with a solvent in which nordiazepam is insoluble in

Going for a bigger run next week and then continuing on with the rest of the procedure.

First run was .23g, this run was 2.3g and the next will be 20g. Will keep you guys posted and will write a report with videos once Im done with the full synthesis
 

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Agilent1100DAD

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@G.Patton

New Update:

Part I out of III, batch 003 (conversion to nordiazepam)

Procedure Used:

"To a vigorously stirred of 2-amino-5-chloro benzophenone (6.93 g, 1 mmol), chloroacetyl chloride (35.8 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 (6.85 g, 3 mmol) and K2CO3 (12.5 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 (300 mL) was added and the product was filtered off, washed with more water (2x 500 mL) and dried. The product was obtained in high yield and purity (94 % yield)"


Interesting enough, the more I scale up, the more yellowish the nordiazepam is.

Anyways, I used the rest of my chloroacetyl chloride (500mL is getting overnighted) up in order to produce the nor diazepam. Something strange happened...usually the solution is a pale yellow, but this time the solution was a red-orange color. The solution solidified! Perhaps all the chloroacetyl chloride was used up? Nonetheless, I proceeded with the wash. I ended up with a yellowish crystalline powder, which still has the right melting point. Im waiting on the Dragendorffs reagent spray to arrive, it will make the TLC analysis much easier. I ended up with 20 g of nordiazepam from the afromentioned batch (003) and a total of 15.3 g from Batch 01-003

Part II out of III, batch 002 (acetylation of nor diazepam)

Procedure Used for batch 002:

"To a vigorously stirred mixture of nordiazepam (1) (2.7 g, 1 mmol), a powder mixture of K2CO3 (5.5 g, 4 mmol)/KOH (2.2 g, 4 mmol) and acetic anhydride (excess 40 mL, 2 mmol) was added. The progress of the reaction was monitored by TLC. After completion of the reaction (3 h), water (3x100 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, with 3x20omL water washes in more than 80 % yield with high purity. The product was used in the next step without any purification."



Batch 001 for Part II was 1/10 of the scale for batch 002, its a simple procedure. My lab tech forgot to put the filter paper on the fritted funnel and some product went through. We re ran the water back into the filter. I am not too happy with batch 001, I see foreign material in the compound and the yield was very low (40%).

Batch 002: I am letting this run overnight.

Conclusion: Once I collect 20 g of the acetylated nordiazepam, I will begin to convert this into alprozolam. Full report with video instructions coming soon

*The two photos added are the comparison between Part I, batch 002 and 003. Batch 002 was yellow and stayed in solution, while batch 003 was a dark orange color and solidified.
 

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Agilent1100DAD

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@G.Patton

New Update:

Part I out of III, batch 003 (conversion to nordiazepam)

Procedure Used:

"To a vigorously stirred of 2-amino-5-chloro benzophenone (6.93 g, 1 mmol), chloroacetyl chloride (35.8 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 (6.85 g, 3 mmol) and K2CO3 (12.5 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 (300 mL) was added and the product was filtered off, washed with more water (2x 500 mL) and dried. The product was obtained in high yield and purity (94 % yield)"


Interesting enough, the more I scale up, the more yellowish the nordiazepam is.

Anyways, I used the rest of my chloroacetyl chloride (500mL is getting overnighted) up in order to produce the nor diazepam. Something strange happened...usually the solution is a pale yellow, but this time the solution was a red-orange color. The solution solidified! Perhaps all the chloroacetyl chloride was used up? Nonetheless, I proceeded with the wash. I ended up with a yellowish crystalline powder, which still has the right melting point. Im waiting on the Dragendorffs reagent spray to arrive, it will make the TLC analysis much easier. I ended up with 20 g of nordiazepam from the afromentioned batch (003) and a total of 15.3 g from Batch 01-003

Part II out of III, batch 002 (acetylation of nor diazepam)

Procedure Used for batch 002:

"To a vigorously stirred mixture of nordiazepam (1) (2.7 g, 1 mmol), a powder mixture of K2CO3 (5.5 g, 4 mmol)/KOH (2.2 g, 4 mmol) and acetic anhydride (excess 40 mL, 2 mmol) was added. The progress of the reaction was monitored by TLC. After completion of the reaction (3 h), water (3x100 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, with 3x20omL water washes in more than 80 % yield with high purity. The product was used in the next step without any purification."



Batch 001 for Part II was 1/10 of the scale for batch 002, its a simple procedure. My lab tech forgot to put the filter paper on the fritted funnel and some product went through. We re ran the water back into the filter. I am not too happy with batch 001, I see foreign material in the compound and the yield was very low (40%).

Batch 002: I am letting this run overnight.

Conclusion: Once I collect 20 g of the acetylated nordiazepam, I will begin to convert this into alprozolam. Full report with video instructions coming soon

*The two photos added are the comparison between Part I, batch 002 and 003. Batch 002 was yellow and stayed in solution, while batch 003 was a dark orange color and solidified.
hello1321Forgot to add the photo for Part I Batch 003, just to compare colors.
 

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catmando

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Forgot to add the photo for Part I Batch 003, just to compare colors.
Agilent1100DADWell done on this, truly excellent work.

I can't get past the first step of this synthesis, I keep ending up with an off white powder MP 118 to 121 which I take is 2-(chloroacetamido)-5-chlorobenzophenone.

Have you got any pointers for me of where I could be going wrong please?

Your help would be greatly appreciated.
 

Hank Schrader

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I would do the first acylation step in cyclohexane.
By mixing 2-amino-5-chloro benzophenone in cyclohexane and slowly dropping chloroacetyl chloride.


You have written in the method
chloroacetyl chloride (1.2 mL, 2 mmol)
1.2ml of chloroacetichloride is 1.7016g which is not 2mmol.
The molar mass of chloroacetichloride is 112.94.
The ideal ratio for acylation per 1 mol of chloramine is not more than 1.26 mol of chloride in the presence of a solvent.
The presence of a solvent makes it possible to control the temperature and obtain a good yield due to temperature stability and the absence of gumming.

I would carry out the cyclization step in dry methanol with urotropine.
 

Agilent1100DAD

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I would do the first acylation step in cyclohexane.
By mixing 2-amino-5-chloro benzophenone in cyclohexane and slowly dropping chloroacetyl chloride.


You have written in the method
chloroacetyl chloride (1.2 mL, 2 mmol)
1.2ml of chloroacetichloride is 1.7016g which is not 2mmol.
The molar mass of chloroacetichloride is 112.94.
The ideal ratio for acylation per 1 mol of chloramine is not more than 1.26 mol of chloride in the presence of a solvent.
The presence of a solvent makes it possible to control the temperature and obtain a good yield due to temperature stability and the absence of gumming.

I would carry out the cyclization step in dry methanol with urotropine.
Hank SchraderExcellent, thank you very much for the cyclohexane advice. Will try this out once my new shipment of chloroacetyl chloride arrives.

XYv1KQbciV

Now for your second suggestion (methanol with urotropine), are you referring to the cyclization step in part I (after the addition of the chloroacetyl chloride) or part III?
 

catmando

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I would do the first acylation step in cyclohexane.
By mixing 2-amino-5-chloro benzophenone in cyclohexane and slowly dropping chloroacetyl chloride.


You have written in the method
chloroacetyl chloride (1.2 mL, 2 mmol)
1.2ml of chloroacetichloride is 1.7016g which is not 2mmol.
The molar mass of chloroacetichloride is 112.94.
The ideal ratio for acylation per 1 mol of chloramine is not more than 1.26 mol of chloride in the presence of a solvent.
The presence of a solvent makes it possible to control the temperature and obtain a good yield due to temperature stability and the absence of gumming.

I would carry out the cyclization step in dry methanol with urotropine.
Hank SchraderHow many ml of methanol per gram of benzophenone would would you add say 5ml per gram?
And how much hexamine?

I've attempted the first part of this synthesis a good few times with the same results, an off white powder with m.p. ranging from 118 to 121.

I had given up on this synthesis but after revisiting this thread and seeing the excellent advance agilent1100DAD made I'm going to give it another shot.

I found the "gumming up" of the solvent less mix very difficult to work with, hopefully some alcohol will help.

So just to clarify after the addition of chloride to benzophenone add methanol, potassium carbonate, ammonium acetate and hexamine?
 

Agilent1100DAD

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Just wanted to update you all; I managed to work some magic and get these incredible off white, long crystals. I’ve increased the starting material from .200 g to 20 g. I’ll be receiving a 5L reaction vessel tomorrow! Very excite

2AvCYJxBVE
2RPFnaSwoi
 

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Agilent1100DAD

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She has finally arrived…

Shes a 5L jacketed borosilicate glass reactor with an addition funnel, condenser, digital RPM controller for the overhead stirrer and temperature gauge. I have it connected to a water reservoir that’s connected to a poly science 1.5 HP chiller with a positive displacement pump and with a temp range of -70C to 300 C.

I am but a speck in an ocean of independent chemists, but this speck is LC-MS validated!!!!!
 

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jarredreyes0303

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cant wait for final results on this one haven't been so hopeful to see someone else succeed in a while. You got this man !
 

TheWaterman

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Are you a buyer of aprazolam. I may have a buyer for few hundred pounds if weed if you have it?
 

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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%.
View attachment 3239
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.
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.
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.
G.PattonWell I for one have a question if manufacturing Alprazolam is so easy and cost effective why is there such a shortage of it?
 
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