4MMC Reagent Kit - First Synthesis (100g Scale)

[xoxoxoxo]

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[Gordon Ramsay]

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xoxoxoxoMaybe try to reload

 

[PsychedelicDog]

Maybe try to reload

Gordon RamsayThe images are uploaded to the tor website they can only be viewed there.

 

[Gordon Ramsay]

The images are uploaded to the tor website they can only be viewed there.

PsychedelicDogMakes sense

 

[xile]

4MMC Synthesis Report (100g 2B4MP)

1. 100g 2b4mp was placed inside of a RBF and 350ml of DCM was added. The solution was stirred for approx. 5 minutes, untill the 2b4mp was fully dissolved in DCM
2. 200ml Methylamine 40% was added in 3 portions (70ml, 75ml, 55ml), every 15 minutes. The temperature started to rise towards 28-30 °C, the colour started to turn slightly yellow
3. The temperature was set to 63 °C so that the RM could reach a temperature of 40°C - 38°C, on the top the temperature remained 30 °C, we assume it is because of the aeqeous layer which already started to form there

4. After 2h of synthesis, 500ml of DH20 was added and allowed to stirr for 5 min. The solution was given 20 minutes to seperate layers, The washing procedure was repeated a total of 4 times, organic layer was kept to proceed.

5. Approximately 175ml of DH2O was added to the previously obtained Meph-Oil (300ml). Stirrer was turned on so that the layers will not seperate

6. ph 5 was reached and the solution was set aside to sepeate layers. The top layer was decanted, the ph of both layers was confirmed.

7. 150ml of Isopropyl 99% have been added to the aeqeous layer of the acidified solution and the solution was heated to 70 °C until slight boiling bubbles showed, the solution was put inside of a glassware dish and locked in a shelf (dark & sealed). Crystalization will take approximately 5 days and the report will be completed once the crystalization was completed.

8. The remaining DCM layer was put into the freezer for 10h as 4MMC remained inside of the DCM layer, when removed a layer of crystals has formed on top (wet weight: 18.41g). It will be put aside for later processing and to learn recrystalization of 4MMC.

View attachment 23144

Gordon RamsayI thought it dosent have to be recrystalated? Your product Look like mine, but it seems like your product is a little dirty. I reach it by toulene. Dcm synthesis never work for me.

Toluene is far easyer since the organic layer remains in separation funnel and with acidify by Aceton give back a realy clean produckt.

After drying you are able to recrystlize imediately.

 

[Gordon Ramsay]

I thought it dosent have to be recrystalated? Your product Look like mine, but it seems like your product is a little dirty. I reach it by toulene. Dcm synthesis never work for me.

Toluene is far easyer since the organic layer remains in separation funnel and with acidify by Aceton give back a realy clean produckt.

After drying you are able to recrystlize imediately.

xileWhen it is coming out of the rotovap, it is dirty I then flush it with frozen acetone one time to let it dry up. Once dried I will clean it further to have a perfectly clean product

What do you mean with recrystalization? I have not recrystalized yet

What was your issue with DCM?

 

[xile]

When it is coming out of the rotovap, it is dirty I then flush it with frozen acetone one time to let it dry up. Once dried I will clean it further to have a perfectly clean product

What do you mean with recrystalization? I have not recrystalized yet

What was your issue with DCM?

Gordon RamsayI can't manage to separate the layers with dcm. I've never had product at the end. With toluene I got the same result as you. But my instructions never mentioned using powder first. It was said that the removed dcm layer (below) is diluted with 100 ml of water and acidified. At ph5, stir vigorously and adjust the ph again. The upper layer of water is then removed and placed in the crystallization dish. According to these instructions you don't get a white or dirty powder, but a viscous brown mass.

Since there is so much color in there I think I didn't separate it properly. But it's too expensive for me to continue working on a method that hasn't achieved anything so far, even though I know a method that I've already successfully used to produce a product.

 

[Gordon Ramsay]

xile Have you checked that with the experts of the forum? Was the colour of your aeqeous layer like that when you decanted it?
Do you have a picture of both layers after acidification? The route worked pretty perfect for me, maybe we can get it to work for you with a few tweaks

 

[Gordon Ramsay]

Crystalization update:

Ca. 25g of dry crastals have been removed (not final yield) from the crystalization dish of the very first synthesis (100g 2B4MP) while we still have liquid left and expect around the same yield once it is fully crystalized

40% - 50% of liquid was left and put back to crystalize, small crystals remained inside of the dish to help crystal growth

The report will be updated once the last crystalization is finished.

 

[Gordon Ramsay]

Crystalization update:

Ca. 25g of dry crastals have been removed (not final yield) from the crystalization dish of the very first synthesis (100g 2B4MP) while we still have liquid left and expect around the same yield once it is fully crystalized

View attachment 23696


40% - 50% of liquid was left and put back to crystalize, small crystals remained inside of the dish to help crystal growth

View attachment 23700 View attachment 23701

The report will be updated once the last crystalization is finished.

Gordon RamsayAs the crystalization dish was filled with up to 1cm the fractions of crystals have turned out quite small compared to the last crystals that had more room to grow.
Another 29.49g of crystals (semi dry) was harvested from the crystalization dish with more liquid remaining. The solution was placed to crystalize again.

The obtained crystals are mainly from a similar fraction as before but smaller, along with salt like 4MMC HCL crystals. The crystals might be from a slightly poorer purity due to a higher concentration of impurities inside of the remaining solution (probably).

So far the total yield of crystals is: 54.6g 4MMC HCL crystals from 100g 2b4mp with more produc to be expected.
I will report on the yield of the other synthesises soon

 

[cascades]

As the crystalization dish was filled with up to 1cm the fractions of crystals have turned out quite small compared to the last crystals that had more room to grow.
Another 29.49g of crystals (semi dry) was harvested from the crystalization dish with more liquid remaining. The solution was placed to crystalize again.

The obtained crystals are mainly from a similar fraction as before but smaller, along with salt like 4MMC HCL crystals. The crystals might be from a slightly poorer purity due to a higher concentration of impurities inside of the remaining solution (probably).

View attachment 24041

So far the total yield of crystals is: 54.6g 4MMC HCL crystals from 100g 2b4mp with more produc to be expected.
I will report on the yield of the other synthesises soon

Gordon RamsayWhere was the precursor 2b4mp & CH3NH2 procured from?

 

[Gordon Ramsay]

Where was the precursor 2b4mp & CH3NH2 procured from?

cascadesHonestly, I don't know But it must have been something good! Yield so far is at 63.48g from 100g 2b4mp and I might be able to squeeze some more out of it. Let's say 65-70g should be max I guess when I have finished all! I will update the report soon

 

[Gordon Ramsay]

Where was the precursor 2b4mp & CH3NH2 procured from?

cascadesOh procured, I read produced. It was from a good contact Telling from the yield the quality was top notch!

 

[byczyborsuk]

Hi. Can you reupload photos please, i see only letters:

 

[MMCHAMSTER]

i hv no idea what you guys are talking about here but does someone know what chemical it is to put inside to get this ultra horny sexuall feeling when doing 4-MMC? xD

 

[JL98]

Still no pictures in the original post, and yes, I use the onion link adress.

 

[Frit Buchner]

My question is, since I'm not hunting the pics down, how does one test the pH of DCM? DCM doesn't have a pH. My litmus papers don't work on non-polar solvents. Can you trust a pH reading that isn't in water?

 

[Johnny_Hammersticks]

My question is, since I'm not hunting the pics down, how does one test the pH of DCM? DCM doesn't have a pH. My litmus papers don't work on non-polar solvents. Can you trust a pH reading that isn't in water?

Frit BuchnerEverything has a ph; if its reading neutral then yore a couple drops away from being slightly acidic. You could get away with the ole red cabbage ph paper with the requirements of this synthesis.

 

[Frit Buchner]

Everything has a ph; if its reading neutral then yore a couple drops away from being slightly acidic. You could get away with the ole red cabbage ph paper with the requirements of this synthesis.

Johnny_HammersticksHilarious kid. Do you know what pH is even an acronym for? Of course you don't or you would understand why only water has pH. Sure other solvents have various amounts of free hydrogen, we call that pK.
I would burN you to the ground with my G.E.D., but it's frowned upon. Stay in school.

 

[Johnny_Hammersticks]

Hilarious kid. Do you know what pH is even an acronym for? Of course you don't or you would understand why only water has pH. Sure other solvents have various amounts of free hydrogen, we call that pK.
I would burN you to the ground with my G.E.D., but it's frowned upon. Stay in school.

Frit BuchnerBased on your response I highly doubt that. Not to many intelligent people get so triggered by a completely innocuous post made by a random stranger on the internet. My apologies that my response to your elementary question hurt your ego to the point of boasting of your failure to attain a high school diploma. So right I can only use my litmus paper to check the ph of polar solvents, thanks for enlightening me. So Im guessing to obtain diluted hcl you of course generated the gas (the only pure form) and then dissolved that into your anhydrous acetone and thats why your litmus paper doesn't read the ph?

Furthermore the ph model can be applied to organic phases that're not aqueous, though not broadly enough to warrant listing. i.e. 1,3 dioxane. Organic conductivity is what bars it from having a readable ph as most have poor conductivity though not all. You state you have litmus paper (which by the way you meant to say "my litmus paper doesn't work on non-polar solvents")

I do not have the same credintials as you with your mighty G.E.D. albeit I'll answer your question; take a sample of your anhydrous immiscible organic phase and mix with water. Stir until equilibrium is reached and then use your litmus paper to determine the ph...dick.

 

[Frit Buchner]

Based on your response I highly doubt that. Not to many intelligent people get so triggered by a completely innocuous post made by a random stranger on the internet. My apologies that my response to your elementary question hurt your ego to the point of boasting of your failure to attain a high school diploma. So right I can only use my litmus paper to check the ph of polar solvents, thanks for enlightening me. So Im guessing to obtain diluted hcl you of course generated the gas (the only pure form) and then dissolved that into your anhydrous acetone and thats why your litmus paper doesn't read the ph?

Furthermore the ph model can be applied to organic phases that're not aqueous, though not broadly enough to warrant listing. i.e. 1,3 dioxane. Organic conductivity is what bars it from having a readable ph as most have poor conductivity though not all. You state you have litmus paper (which by the way you meant to say "my litmus paper doesn't work on non-polar solvents")

I do not have the same credintials as you with your mighty G.E.D. albeit I'll answer your question; take a sample of your anhydrous immiscible organic phase and mix with water. Stir until equilibrium is reached and then use your litmus paper to determine the ph...dick.

Johnny_HammersticksI answered your question you pmed me. I'm a psychopath so I really don't grasp social concepts well. A GED is a "graduate equivalent diploma" if you have a GED, it means you dropped out of school or hadn't graduated by the time you were 18. I don't actually have a GED, I graduated high school, it was an insult. To say someone who didn't graduate is more educated than you. That post was a trap, it gets the noobs because being in water is a prerequisite for having a pH/poh. My litmus paper really doesn't work worth a damn on organic solvents.

 

[Frit Buchner]

Based on your response I highly doubt that. Not to many intelligent people get so triggered by a completely innocuous post made by a random stranger on the internet. My apologies that my response to your elementary question hurt your ego to the point of boasting of your failure to attain a high school diploma. So right I can only use my litmus paper to check the ph of polar solvents, thanks for enlightening me. So Im guessing to obtain diluted hcl you of course generated the gas (the only pure form) and then dissolved that into your anhydrous acetone and thats why your litmus paper doesn't read the ph?

Furthermore the ph model can be applied to organic phases that're not aqueous, though not broadly enough to warrant listing. i.e. 1,3 dioxane. Organic conductivity is what bars it from having a readable ph as most have poor conductivity though not all. You state you have litmus paper (which by the way you meant to say "my litmus paper doesn't work on non-polar solvents")

I do not have the same credintials as you with your mighty G.E.D. albeit I'll answer your question; take a sample of your anhydrous immiscible organic phase and mix with water. Stir until equilibrium is reached and then use your litmus paper to determine the ph...dick.

Johnny_HammersticksYes, I drip HCl water into H²SO⁴, then bubble the gas through my cold trap, filled with more H²SO⁴, which dries the gas. It's the most convenient method for me because it doesn't need heat and the rate is easily adjustable by the petcock on my pe funnel

 

[Johnny_Hammersticks]

I answered your question you pmed me. I'm a psychopath so I really don't grasp social concepts well. A GED is a "graduate equivalent diploma" if you have a GED, it means you dropped out of school or hadn't graduated by the time you were 18. I don't actually have a GED, I graduated high school, it was an insult. To say someone who didn't graduate is more educated than you. That post was a trap, it gets the noobs because being in water is a prerequisite for having a pH/poh. My litmus paper really doesn't work worth a damn on organic solvents.

Frit BuchnerI didn't graduate high school in the traditional sense, and obtained my G.E.D. while serving my first out of 3 bids in the joint, cause I too am a little bit off kilter, lol. I am just fascinated by o.chem and like to party so instead of working research and development for some piece of shit pharmaceutical company I chose to go this route. There is a lot I don't know though and many things I overlook until they're pointed out to me so am always looking to learn whatever I can from whoever is willing to teach me.

 

[Muskett13]

I didn't graduate high school in the traditional sense, and obtained my G.E.D. while serving my first out of 3 bids in the joint, cause I too am a little bit off kilter, lol. I am just fascinated by o.chem and like to party so instead of working research and development for some piece of shit pharmaceutical company I chose to go this route. There is a lot I don't know though and many things I overlook until they're pointed out to me so am always looking to learn whatever I can from whoever is willing to teach me.

Johnny_HammersticksHey I respect this guys motivation AND your reasoning isnt far from the most sane thing to say in justification to your reasoning my friend! I too have the interests and reasoning in the same situations! We should be friends and possibly help eachother from time to time pm me.