Das einfachste Rezept für kristallines Mephedron

[BevItUp]

UWe9o12jkied91d Könnten Sie bitte die Methode näher erläutern, über die Sie und mocnykutas diskutieren?

Vielen Dank

 

[UWe9o12jkied91d]

Ich weiß nicht, mit welchem Verfahren er immer wieder prahlt, aber im Moment habe ich die besten Ergebnisse, wenn ich das Keton in etwas dcm auflöse, leicht auf 35-40 erwärme, das Methylamin auf einmal hinzufüge, 10m rühre und dann nach und nach dmso im Laufe von 20-30min hinzufüge.dann Wasser und etwas Ethylacetat hinzufüge und noch ein paar Minuten rühre, abtrenne.mit kaltem Aceton verdünne und ausfalle, habe ich sowohl 33 als auch 37,5 HCl ausprobiert, kein nennenswerter Unterschied.
Von allen Verfahren, die ich angewandt habe, war dieses am saubersten und ertragreichsten. Und nebenbei bemerkt, ich denke, je größer der Maßstab, desto besser funktioniert es.

 

[dodobird]

Why add the solvent along with water for flushing though? Noob here
What uf starting solvent is EA instead of DCM?

 

[Usernamealready]

Great question! When flushing a column in chromatography, the goal is to remove any residual compounds from the stationary phase to ensure a clean system for the next run. The choice of solvent and whether to include water depends on the properties of the solvents used during the chromatography process.

Why Add Solvent Along with Water for Flushing?

1. Solvent-Solvent Compatibility: Many organic solvents (e.g., ethyl acetate, DCM, hexane) are immiscible with water. If water is used alone, it may not effectively remove nonpolar residues. Adding an organic solvent ensures that both hydrophilic (polar) and hydrophobic (nonpolar) residues are washed out.


2. Effective Column Cleaning: If the mobile phase was a mixture of organic solvent and water (e.g., ethyl acetate/water or MeOH/water), using both in the flush prevents precipitation of residual materials, which can clog the column.


3. Preventing Phase Separation Issues: In some cases, a solvent switch from an organic solvent directly to water can lead to phase separation, causing bubbles or irregular flushing. Using a miscible solvent before introducing water ensures smooth transitions.




---

If Starting Solvent is Ethyl Acetate (EA) Instead of DCM?

Ethyl acetate (EA) is more polar and water-miscible to some extent, whereas DCM (dichloromethane) is less polar and immiscible with water. The flushing strategy changes depending on the starting solvent:

For EA: Since EA is slightly water-miscible, a water wash alone may work to some extent, but using a mix of EA and water ensures better residue removal.

For DCM: DCM is completely immiscible with water, so a transition solvent (like methanol or ethanol) is often used before adding water.


Practical Approach:

If you used EA as the mobile phase, first flush with EA, then follow with a more polar solvent (e.g., methanol), and finally with water.

If you used DCM, first flush with DCM, then use a bridging solvent (MeOH or IPA) before introducing water.


Hope this helps! Let me know if you need more clarification.

 

[dampus66]

Wie soll ich bei geschlossenem Deckel rühren? Muss ich den Deckel zum Rühren abnehmen?

 

[dodobird]

Umm....magnetic stirrer?

 

[Kiteretsu_D]

Hey Leute, ich brauche etwas Hilfe bei der Synthese. Ich wäre euch dankbar, wenn ihr mir ein wenig helfen würdet. Ich bin ein Anfänger in dieser chemischen Sache, aber ich denke, ich verstehe 80% dieses Prozesses, für die anderen 20% brauche ich etwas Hilfe von euch

 

[W.P.3]

Was ist Ihr Problem?

 

[dodobird]

Me too. 10 k 2b4m

 

[alwaysalpha]

Hat jemand dieses Rezept schon einmal ausprobiert???

 

[mrbeest]

Ich bin

 

[alwaysalpha]

Share it

 

[Davidmalik96]

please clarify

 

[frosties]

Where can I buy benzene/Benzol in Germany anonymously?

 

[dnBQByvHb8Zkawbjpx]

Benzene is rather restricted in the EU. You may be able to find a seller but as an individual consumer you'll have a hard time justifying the purchase of more than limited quantity. Ethyl acetate is a solvent for making 4MMC that can be obtained the easiest, is fully legal and not restricted, and is quite cheap.

 

[frosties]

Thx I'll go with you his method.

 

[dnBQByvHb8Zkawbjpx]

Do you have experience with recovering solvents through distillation? DCM is moderately difficult to obtain (restricted for consumers in the EU) and NMP is expensive, so reusing them could be an interesting option.

 

[jango]

Wow, that yield is massive. Are there any alternatives to NMP to work as a phase transfer catalyst? I've read that it could be substituted by DMSO, are there any other options that may be cheaper and more easily available?

I don't understand why solvents are not reused on a larger scale as well - it limits the volume of waste and brings down the cost.

 

[dnBQByvHb8Zkawbjpx]

Wow, that yield is massive. Are there any alternatives to NMP to work as a phase transfer catalyst? I've read that it could be substituted by DMSO, are there any other options that may be cheaper and more easily available?

I don't understand why solvents are not reused on a larger scale as well - it limits the volume of waste and brings down the cost.

 

[61-50-7]

Some impurities stay in the solvent so distillation is needed for reuse and it takes a lot of time and need large equipments. For legal businesses it's possible but for drugs way more complicated (time, space, electricity consumption, etc)

 

[dnBQByvHb8Zkawbjpx]

I understand that and I had distillation in mind to recover pure solvent. Especially DCM with its boiling temperature of 40 °C requires almost no energy to distill. I'm definitely going to do that and in about a month I should have some first-hand experience to share.

 

[dodobird]

Hi. This post made months of reading confusion go away, very straightforward, thanks @Madre . I had some important doubts to be cleared for upcoming MasterChef tryout , appreciate guidance on them. Here we go...

1. Can I replace the benzene with say 300 ml Ethyl acetate. If so what proportion would be ideal and if any procedural changes needbto be made, I am guessing not.

2. Is it Hcl38% we should use?

3.Does the methyl gad need to be relased after animation at all or do we just pour it in shake and then seal to put in the fridge?
How can I reduce this stage to under 1 hour or 2. Any temperature rise monitoring or precaution until this stage? Max temp?

4. Do we need to was the freebase during flushing, with nac03 plus water first and then 2 x with distilled water?

5. Is this method of preparing the 10-90 Acetine hcl38 solution and adding together, better yielding or beneficial over the much common separate addition method of acetone and hcl38? Does it affect quality potency or failure chances or perhaps yield weight of final powder 4mm

6.... Please share equationally correct reagent and chemical quantities for making 10 kg a day. Also any simple apparatus methods for doing this quantity without much labware beside basic flask and jar. What reaction container could I probably use to replace a reactor etc etc


THANKS YOU VERY MUCH IN ADANCE , GREA JOB!!!

 

[Usernamealready]

There are so many methods mentioned in it that I am confused. There are so many chemicals mentioned. So many things. Which method should I follow?

 

[Usernamealready]

hello sir
how are you?I have 5 KG P2P and 5 KG Methylamine.Can we proceed now?