Methylphenidate (Ritalin) synthesis

[cokemuffin]

Would you get other esters of ritalinic acid if you'd do the last step in other solvents (IPA = isopropylphenidate, EtOH = ethylphenidate etc.)?

 

[G.Patton]

Hi, yes, you will.

 

[cokemuffin]

What do you mean with 4f, i can not follow you?

 

[G.Patton]

Hi. NaOH in IPA will completely spoil your ritalin*HCl. You can get ritalin freebase by aqueous NaOH and then carry out esterification.

 

[cokemuffin]

So would the process be to put the ritalin hcl in NaOH solution, get the ritalin freebase and then just put that in ipa to get isopropylphenidate? I'd guess the hcl should be added after esterfication to not replace the OH from the carboxyl group with a Cl, but i'm not 100% sure about that.

 

[G.Patton]

Hello, sorry for a long reply. I haven't seen you question.
No, eterefication isn't work like you describe. You have to get Ritalinic acid sodium salt and then get ester with IPA in acidic condition.
It won't work like you told =) What is a reason for these manipulations? Actually, I'm not sure that reaction will be sucsess. Moreover, you'll loose part of your ritalin.

 

[cokemuffin]

Never looked into eterefications, but if doing full synthesis appears to be the only viable option anyways, i guess i don't even have to. Instead i searched a bit more for routes to get methyl phenylglyoxylate. Thought about getting it from benzoyl chloride might be a good option, but i've only found syntheses that involve cyanides. Gringard reagents instead of cyanides would make it much safer but for some reason i couldn't find a synthesis of the reaction beneath anywhere?

I guess you could just replace benzyl chloride with benzoyl chloride and do the same reaction as you'd do to get PAA, but i'm not sure if there's something interfering.

 

[G.Patton]

Hello, there is oxygen. You can't carry out such synthesis.

 

[cokemuffin]

Fuck, now i at least know it interferes. benzoyl chloride and CuCN is the only way from benzoyl chloride then?

 

[G.Patton]

For what? It is not PAA (phenylacetic acid).

 

[cokemuffin]

Ik, if you use benzyl chloride instead in the reaction above it gives you PAA. Thought using benzoyl chloride instead of benzyl chloride will give phenylglyoxylic acid, but since the oxygen interferes in the reaction the only way i know instead would be to use cyanides instead:

 

[TheNut22]

When syntheses involves cyanides, I go to my local hardware store pool-chem section and by Na DCCA, or TCCA. They will do the same reaction as more poisonous cyanide forms. I've made so many times phenylacetic acid from DLPA, and so on ..

 

[Lordoftheshard]

I no this is a bit off topic I have a friend who has stick piled these tabs 10 mg
He asked me if there is any way you can extract the ritalin out of the tabs and make it into a smoke able form like meth

 

[G.Patton]

Hi, acid/base extraction

 

[Lordoftheshard]

Thankyou sir as I tried normal Extractions first with ethanol doesn't matter if you filter and so forth end up blockers and other junk#. Coming over with it buy coincidence I seen your thread and though I would ask and brother thankyou this is the only way you can extract ritalin clean and properly I looked on Reddit and so forth I haven't seen any one elses as clean as this

 

[G.Patton]

Amphetamine purification by acid-base extraction I told about acid-base extraction, it is different procedure than you did. Read about it in this topic. Also, you can read about extraction procedure theory to understand what are you doing: Extraction

 

[Lordoftheshard]

I first dyd alcohol extracting bug blockers etc kept coming over with it
Then I did ab extraction to get this

 

[Lordoftheshard]

Thankyou

 

[toffifee]

Hello everywhere, can you help me find a marketplace to buy 1-Phenyl-2-(piperidin-1-yl)ethanone-1,2-dione. or Methyl phenylglyoxylate ? What is the best website for ordering reagents and laboratory equipment? CIS countries

 

[blackshwan]

Hello @G.Patton .


About this step (refluxing).
[The reaction mixture was gently refluxed for 3-12 hours with reflux condenser (as determined by monitoring by TLC). ]


What is the temperature of the heat souce? Thanks.

https://bbgate.com/attachments/lwndic7fo8-png.2904/

What is "heating under reflux"?

When dealing with organic reactions, heating under reflux is often required, such as the oxidation of Toluene using acidified $\ce{KMnO4}$ and dilute $\ce{H2SO4}$ to Benzoic acid($\ce{C6H6O2})$ What

chemistry.stackexchange.com

 

[G.Patton]

Hello. The temperature, which would be enough to boil the mixture of 1-phenyl-2-(piperidin-1-yl)ethane-1,2-dione (1) in dimethoxyethane was added p-toluenesulfonhydrazide (2) (1.1 equivalent) at normal conditions (22*C, 760 mm Hg).

 

[dupskoslonia]

Hey guys. I have ritalinic acid. What do I need to make metylphenidate and etylphenidate? I'm a complete newbie, could you please explain me step by step? Would be really grateful

 

[HerrHaber]

You need to convince your carbonyl group to make an ester with methanol and ethanol respectively. This is pretty straight forward by standard chemical means and try looking for rather mild methods such as enzymes (lipases) or easy to work with ClSiMe3 in methanol with substrate.

 

[kotkata]

Is there a protocol or beginner's guide or recipe of some sort to convert ritalinic acid to methylphenidate?

To my understanding it's not rocket, but I'm a bit confused how to get methylphenidate from ritalinic acid.

 

[kotkata]

Awesome, thank you so much, @dupskoslonia!

Really appreciated!!

 

[untryrgos]

Hi, thank for your synthesis way.I follow your way and some difference appeared.when I make sure all acid disappear and finished first step,I found so much salt separation. Is it the Methylphenidate sulfate? The pH is about 1 to 2.