Did I just cook up a complete disaster?

[katharina]

Hi
I was doing the synthesis of 5f-adb and I think I fucked big time.

I think my stir bar in the magnetic stirrer was a bit too big (35mm compared to the default 30mm from the set, which I lost once) - it did create a fairly strong vortex, but its trajectory was strange and unsteady. It stayed fairly in the middle all the time. It was just a bit shaky i guess. I did everything according to the
instructions, set the temperature to 78 degrees (I didn't want to overheat, and I don't know how much I can trust the probe with the thermometer from the magnetic stirrer set) and maintained the temperature for 5h while stirring. Then I let the liquid cool to room temperature - and here the first problem and question. While waiting, unfortunately, I fell asleep for about 3h. After waking up, the temperature was room temperature, but I don't know if something bad happened during that time. Is that possible?

Anyway, after waking up and inspecting the substance, I noticed that there was a lot of undissolved powder at the bottom, with one fairly large clump. I tried to gently stir it with a glass rod, but it didn't make much sense, so I proceeded to the next step. And here the real troubles begin.

For the next step, I used an overhead stirrer. After pouring the liquid into ice water while stirring, a sticky, rubbery, homogeneous mass started to accumulate around the stirrer blade, which at some point built up so significantly that it started blocking the blade. Somehow I managed to finish, but after that it looks like this:

Currently, I'm at the stage of cooling it in the fridge for another 5h, but I have no idea if this even makes sense at this point.

 

[G.Patton]

>>>While waiting, unfortunately, I fell asleep for about 3h. After waking up, the temperature was room temperature, but I don't know if something bad happened during that time. Is that possible?
Hi, it's okay.

>>>For the next step, I used an overhead stirrer. After pouring the liquid into ice water while stirring, a sticky, rubbery, homogeneous mass started to accumulate around the stirrer blade, which at some point built up so significantly that it started blocking the blade. Somehow I managed to finish, but after that it looks like this:

It's also ok. Let it completely dry. It's worth to use vacuum desiccator for this.

 

[katharina]

Wow, thank you so much. You’ve really calmed me down. Could you also shed some light on the issue of the “undissolved” powder that remained at the bottom after 5 hours of mixing? Is that normal, or could the slightly irregular vortex have caused the substance to mix unevenly, resulting in that residue?

 

[G.Patton]

I can't answer you for sure. In my assumption, there are two options:
1. Undissolved precursor due to weak stirring
2. Final product, which has formed these lumps.

 

[katharina]

Do you have any idea how can it affect the quality or final amount of the product? Is it safe to use?

 

[G.Patton]

I would recommend you to try purification method as in this topic. Try this with a small part like 3-5g. If it will be ok, repeat with other part.

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/en/threads/5-cl-adb-a-mdmb-4en-pinaca-synthesis.15239/

 

[katharina]

II'm afraid I don't have required equipment to do so.

 

[karmahdelic]

Ola, o que não dissolveu completamente foi o carbonato de potássio. Se não estiver em pó fino ocorre esse problema , pois às vezes pode vim micro compactadores. Tive esse problema de sobra de resíduos no fundo do Becker.

Quando foi pro gelo aconteceu a mesma coisa e ficou essa gosma ( eu despejei todo conteúdo do Becker até o material que não dissolveu) quando terminei de bater no gelo acrescentei mais 5kg de gelo e misturei devagar algumas vezes e ele foi começar a solidificar depois de 1 hora , aí foi quebrando e separando os pedaços para facilitar na cristalização

 

[RCBOSS888]

The powder that hasn't completely dissolved is likely undissolved Potassium carbonate, which is normal—no need to worry about it.
To ensure you cook get better finished product, I recommend you switching to the Overhead stirrer instead of a magnetic stirrer.