Second step Leuckart amination(large scale)

[Selassi]

Swim got a question regarding a different variation on this classic method:

After the first step (boiling with formic and formamid), they now directly boil again the organic phase with water and NaOH instead of the classic reflux with HCl and after NaOH.

After this step steamdistill is used ofc.

Can someone explain to me the metrics on this different second step to me? Swim has never done it this way but it seems to save a lot of time in contrast to the oldschool method with refluxing HCl.

What strength of caustic/water and how much is introduced to the reactor per L of product?
How long should swim boil this reactionmixture at what temp?

 

[G.Patton]

Hello, Selassi. There are answers to your questions. You can count amounts proportionally for 1L, if you need.

 

[Selassi]

Hello bro
i have read this thread but thats not what i mean.
They skip all of those steps given in the method u linked

From p2p to A they now use just 2 steps before steamdistillation
Step 1 boil formic and formamid
Throw away watery phase
Step 2 boil with NaOH
Throw away watery phase
Step 3 steamdistill

This second step i mean

 

[Bartholomeus]

From where do you have this information?
From someone who is really producing and you trust?
How can they omit the Hydrolysis step with HCL and go directly to NaOH?
NaOH is there only to raise ph and participate the freebase a oil from reaction so you can then proceed to distill it from reaction

@William Dampier @btcboss2022 @G.Patton do you guys have any info in this method OP is asking about?

 

[btcboss2022]

The method is correct in the proper amounts times and temperatures.

 

[Selassi]

Exactly, its used in large scale operations and will save a lot of time, risk and money...
So i see this method is not well known here...

 

[studentt]

what is the amount of formic and formamide you put on 1 liter p2p?

 

[G.Patton]

He told about William D. posted method.

 

[Bartholomeus]

Can anyone please write ratio for p2p/formamide/formic
And then how much NaOH after the first step

 

[Selassi]

U mean this variation method as stated above or the method William described?

 

[studentt]

Can anyone please write ratio for p2p/formamide/formic
i use this methode also can somebody write how much acid and formamide, and by step 2 how much hcl with the oil

 

[Selassi]

Thats given in the method from William i believe.
The point of this variation is to skip the HCl reflux.

 

[G.Patton]

Hi. Please, stop spam and open my link above and read article. There are answers.