sticky mass

[Aney]

how to deal with sticky mass which produced during organic synthesis ?

[hypervalent_iodine]

Could you elaborate? Is this the final product following work up? Deal with how?

[Aney]

it is building block for synthesis of the final products

I want to make it as powder to complete my work

any idea for helping ???

[hypervalent_iodine]

Is it meant to be a powder? Sometimes you just have to work with what you’ve got. It shouldn’t matter too much that it’s a sticky solid, unless the fact that it’s sticky is because it contains impurities. 

[Sensei]

8 hours ago, Aney said:

how to deal with sticky mass which produced during organic synthesis ?

If you meant "how to separate chemical compounds?", you should start from reading this article and its links:

https://en.wikipedia.org/wiki/Separation_process

It should give you brief idea which procedures are available.

 

Edited December 13, 2018 by Sensei

[Aney]

9 hours ago, hypervalent_iodine said:

Is it meant to be a powder? Sometimes you just have to work with what you’ve got. It shouldn’t matter too much that it’s a sticky solid, unless the fact that it’s sticky is because it contains impurities. 

It is recommended to be solid powder, because of my fearing that impurities make it as sticky mass not powder ..

10 hours ago, Sensei said:

If you meant "how to separate chemical compounds?", you should start from reading this article and its links:

https://en.wikipedia.org/wiki/Separation_process

It should give you brief idea which procedures are available.

 

O. K

[hypervalent_iodine]

Have you run any NMR or GCMS? 

[Aney]

1 hour ago, hypervalent_iodine said:

Have you run any NMR or GCMS? 

No ..

[hypervalent_iodine]

I would suggest you do that so you can figure out what you have first. 

[John Cuthber]

There are two options.

Use the stuff as it is to make your final product (in which case the product will need cleaning up)

Clean up this intermediate- which will give you a product that's cleaner- but will still need cleaning up to get a pure material.
The second course of action will probably give a better product, but the yield will be lower.
It's more or less traditional in chemistry that you have that trade -off. You can have high purity  or high yield, but not (usually) both

[Aney]

On 12/15/2018 at 4:49 AM, John Cuthber said:

There are two options.

Use the stuff as it is to make your final product (in which case the product will need cleaning up)

Clean up this intermediate- which will give you a product that's cleaner- but will still need cleaning up to get a pure material.
The second course of action will probably give a better product, but the yield will be lower.
It's more or less traditional in chemistry that you have that trade -off. You can have high purity  or high yield, but not (usually) both

Nice speech ..

On 12/14/2018 at 4:40 PM, hypervalent_iodine said:

Have you run any NMR or GCMS? 

No ..

[hypervalent_iodine]

Also worth noting that some reactions tolerate impurities better than others, so I would again recommend that you at least figure out what’s in there first. Can I ask what you’re making?

[Aney]

1 hour ago, hypervalent_iodine said:

Also worth noting that some reactions tolerate impurities better than others, so I would again recommend that you at least figure out what’s in there first. Can I ask what you’re making?

I will go ahead to the next reaction using the same sticky mass because NMR and MS take long time to be done ..

[hypervalent_iodine]

That is not a great attitude. NMR and MS really take very little time, assuming you have access to the facilities. Certainly a lot less compared to how long it may take you to redo your reaction if it doesn’t work out because you didn’t want to invest an hour or two in doing some very standard checks. Where has this sticky mass of yours come from? Did you make it? 

[John Cuthber]

13 hours ago, hypervalent_iodine said:

That is not a great attitude. NMR and MS really take very little time, assuming you have access to the facilities

And if that assumption is invalid...?

[hypervalent_iodine]

Their previous post indicates that they have access, but I am not sure if it is administered as a walk-up or as a service operated by a technician. The latter would likely have longer wait times for results. Regardless, I think in the long run you end up wasting more time proceeding with a reaction if you don’t actually know for sure what is going into it. Depending on how precious this compound is and how complicated the reaction they’re doing is, you could probably get away with doing a test run on small scale and seeing how the reaction tolerates it. Even then, figuring out if it worked could be made more difficult by the added impurities, if the ‘sticky mass’ is even the compound they want and not just a decomposed mess, or something stemming from a bad synthesis. 

[BabcockHall]

I hesitate to jump in without knowing more.  On occasion a sticky mass can be made more tractable through trituration.  Perhaps a different purification technique would be more suitable.