• Welcome to the forum of professional participants of the drug market!

    Here you will get all the necessary information about organizing a laboratory of any size, from a small kitchen at home to an industrial facility.
    And if you have your own production, here you will find all the relevant information to improve efficiency and safety.
    In the sections of the forum you will find:

    • Methods of synthesis and analysis;
    • Suppliers of chemicals and equipment;
    • Descriptions of the pharmacological action of substances;
    • Business technologies.

Ketamine synthesis

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
736
Reaction score
431
Points
63
No, In this reaction you don't need it. Sorry for first misleading.
 
Last edited:

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
No, In this reaction you don't need it. Sorry for first misleading.
Yes,sir.I would like to ask in part 9,do I need to heat the CCI4 after cleaning it with Sodium bisulfite?Also is there a need to add a desiccant to turn it into a powder at the end?Like the one at the end of part 8.
 

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
736
Reaction score
431
Points
63
Saturated with methylamine in step 10,what is its CAS No?
cas 74-89-5 or CAS 593-51-1 and use procedure from step 10 to get methylamine gas.
Yes,sir.I would like to ask in part 9,do I need to heat the CCI4 after cleaning it with Sodium bisulfite?Also is there a need to add a desiccant to turn it into a powder at the end?Like the one at the end of part 8.
Where did you read about sodium bisulfite in this step? You don't need to use desiccant.
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
cas 74-89-5 or CAS 593-51-1 and use procedure from step 10 to get methylamine gas.

Where did you read about sodium bisulfite in this step? You don't need to use desiccant.
Sorry,Is it necessary to heat after washing with sodium bisulfite after the orange suspension formed in step2?
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
Sir, I would like to ask In the first step,when Cyclopentylmagnesium bromide and 2-Chlorobenzonitrile are stirred for 3 days,what will be the reaction to know the completion of the step?Also what is the ratio of NH4CI to reactant?Also what is the ratio of benzene to reactant?
 

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
736
Reaction score
431
Points
63
Sorry,Is it necessary to heat after washing with sodium bisulfite after the orange suspension formed in step2?
What don't you understand there? or what do you want to heat? You have to wash the reaction solution with aq sodium bisulfite and than evaporate organic solution. This washing reduce amount of bromine excess
This is washed with a dilute aqueous solution of sodium bisulfite and evaporated to give 1-bromocyclopentyl-(o-chlorophenyl)-ketone, bp 111-114 °C (0.1 mm Hg).
Sir, I would like to ask In the first step,when Cyclopentylmagnesium bromide and 2-Chlorobenzonitrile are stirred for 3 days,what will be the reaction to know the completion of the step?
You can set a timer for 72 hours or use TLC to check reaction completion.
Also what is the ratio of NH4CI to reactant?
I already answered you.
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
What don't you understand there? or what do you want to heat? You have to wash the reaction solution with aq sodium bisulfite and than evaporate organic solution. This washing reduce amount of bromine excess


You can set a timer for 72 hours or use TLC to check reaction completion.

I already answered you.
Sir,Thank you for teach!
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
What don't you understand there? or what do you want to heat? You have to wash the reaction solution with aq sodium bisulfite and than evaporate organic solution. This washing reduce amount of bromine excess


You can set a timer for 72 hours or use TLC to check reaction completion.

I already answered you.
Sir, I would like to ask at the end of the part 8,what is the ratio of benzene to reactant.Also in part 2,what is the ratio of sodium bisulfite to reactant?
 

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
736
Reaction score
431
Points
63
Sir, I would like to ask at the end of the part 8,what is the ratio of benzene to reactant.Also in part 2,what is the ratio of sodium bisulfite to reactant?
8. o-Chlorophenyl cyclopentyl ketone.
To the thus obtained Grignard soln there’s added 48 g o-chlorobenzonitrile and the mixture is stirred for 3 days at RT. It is then poured into a mixture of ice/NH4Cl, with addition of some conc. aq. NH3 and left at ambient temp until all ice melts. The ketone partially floats, partially goes to the bottom. It’s extracted with benzene (Use 100 mL x2 times). The yields fluctuate, but rarely drop below 55%.

Step 2: alpha-bromo (o-chlorophenyl)-cyclopentyl ketone.
To 21.0 g of the above ketone is added 10.0 g of bromine in 80 ml of carbon tetrachloride dropwise at 0 °C. After all the Br2 has been added, an orange suspension forms. This is washed with a dilute aqueous solution of sodium bisulfite (~65 mL x2 of 10% solution) and evaporated to give 1-bromocyclopentyl-(o-chlorophenyl)-ketone, bp 111-114 °C (0.1 mm Hg). Yield is ~66%. This bromoketone is unstable and must be used immediately. Also, attempts to distill it at 0.1 mm Hg lead to some decomposition, so it should be used without further purification.
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
8. o-Chlorophenyl cyclopentyl ketone.
To the thus obtained Grignard soln there’s added 48 g o-chlorobenzonitrile and the mixture is stirred for 3 days at RT. It is then poured into a mixture of ice/NH4Cl, with addition of some conc. aq. NH3 and left at ambient temp until all ice melts. The ketone partially floats, partially goes to the bottom. It’s extracted with benzene (Use 100 mL x2 times). The yields fluctuate, but rarely drop below 55%.
Sir,this question seems silly,but for the novice I still want to ask in detail,during the extraction process,the reactant and benzene,which one should precipitation and which one should float?
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
Step 2: alpha-bromo (o-chlorophenyl)-cyclopentyl ketone.
To 21.0 g of the above ketone is added 10.0 g of bromine in 80 ml of carbon tetrachloride dropwise at 0 °C. After all the Br2 has been added, an orange suspension forms. This is washed with a dilute aqueous solution of sodium bisulfite (~65 mL x2 of 10% solution) and evaporated to give 1-bromocyclopentyl-(o-chlorophenyl)-ketone, bp 111-114 °C (0.1 mm Hg). Yield is ~66%. This bromoketone is unstable and must be used immediately. Also, attempts to distill it at 0.1 mm Hg lead to some decomposition, so it should be used without further purification.
Sir,You said 65ml*2 for cleaning.Do you need to add sodium bisulfite to repeat the evaporate twice?Or do you mean130ml for one?
 
Last edited:

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
736
Reaction score
431
Points
63
Sir,this question seems silly,but for the novice I still want to ask in detail,during the extraction process,the reactant and benzene,which one should precipitation and which one should float?
benzene has lower density hence it will on top
Sir,You said 65ml*2 for cleaning.Do you need to add detergent to evaporate twice?Or do you mean130ml?
You got reaction mass after reaction and there is excess of Bromine. You add water solution of sodium bisulfite to reaction mass, shake it, divide layers. Repeat procedure. You have to discard water layer (with sodium bisulfite) after washing. NaHSO3 bounds excess bromine from reaction mixture after reaction. Do you understand?
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
You got reaction mass after reaction and there is excess of Bromine. You add water solution of sodium bisulfite to reaction mass, shake it, divide layers. Repeat procedure. You have to discard water layer (with sodium bisulfite) after washing. NaHSO3 bounds excess bromine from reaction mixture after reaction. Do you understand?
Do I need to repeat the wash and evaporate 2 times?
 

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
736
Reaction score
431
Points
63
So i am going to continue experimenting with the bottom?
No, your extraction with benzene means that your product will be extracted (located in benzene) by benzene. Than you will work with extract (benzen+product).
Do I need to repeat the wash and evaporate 2 times?
no, you have to evaporate sln. after both washing procedures...
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
No, your extraction with benzene means that your product will be extracted (located in benzene) by benzene. Than you will work with extract (benzen+product).
Thank you for your detailed explanation,I understrand.
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
no, you have to evaporate sln. after both washing procedures...
Do you mean washing the reactant 2 times and then heating and evaporating 1 more time to get the product?
 

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
736
Reaction score
431
Points
63
Do you mean washing the reactant 2 times and then heating and evaporating 1 more time to get the product?
Only once, no more. Do you understand procedure? Read several times to understand better. I have already written this info. There is clearly detailed explanation.
 

joejoe

New member
Premium
Joined
Aug 1, 2022
Messages
23
Reaction score
2
Points
3
Only once, no more. Do you understand procedure? Read several times to understand better. I have already written this info. There is clearly detailed explanation.
Sir,I will try to find out.
 
Top