First time 4mmc synth assistance

[dodobird]

For the initial demo run to show the contracting party i plan to use
2b4m 250 gms dissove it in Ethyl acetate 1000 ml in a 3 neck flask, keeping temp below 60 deg with a cold water bath. Add 500 ml of aq ma 40% in 2 or 3 parts while shaking/stirring. Either shake manually or might use a mag stirrer if available. From what i read, i might need to gently heat to about 40-45 deg c to achieve the desired color of crude 4mmc in Ea(should it be dark yellow or brown?). Leave alone for 2 hours.
Once visible freebase layer visibly forms and separates, drain ea ma layer which should be at the bottom.
Add 1000 ml of naco3 plus distilled water and wash the freebase once after stir/shake/swirl ( does the flask need to be sealed or open here).
Wash 2x or 3x with d water until no fishy or ma smell.
Add 500 ml chilled dry acetone (is this regular acetone), stirring while doing this.
Add chilled hcl 38 drop wise until litmus shows exactly between the yellow and orange. (Please let me know which exact color shows ph5.5?).
Stir a couple of minutes, take off and cover this beaker using a cling wrap or sanwich plastic. Place at about 10dg for an hour then in freezer 1dg for an hour or two.
Filter this with cold acetone until almost white salt remains . Leave pump on for 20 minutes so all liquid drained.
Recrystallize using 30ipa 70h20 solution in parts.
Appreciate any remarks feedback shortcuts corrections and guidance to enable this humble first timer to nail it nicely and chalk one up for the bbgorum.

I have the procedure set in my mind but a step by step here using minimal lab eq and no extra reagents would be bolstering ny self belief.
I want to synthesize quality and potent 4mmc withing the shortest time period.

Thanks in advance.

 

[Berlin777]

Why cold water bath if you dissolving 2b4mp?

 

[dodobird]

Sorry bout that you're right my text edit was incorrect. Add ea n heat no bath here but next step with ma

 

[William D.]

Tell us where you read this method?

 

[dodobird]

I've gathered this from various posts.. appreciate constructive criticism if you would be so kind

 

[William D.]

(click) - this is not the best synthesis, but you see better in the video. This is easier than you think.
(click) - here you can see in more detail on other equipment

 

[dodobird]

The Voss method was my first choice but couldn't get 4mp
Please point out the flaws in mybtheoretical method above. Would be eternally obliged

Are the measurements off and if so for which part.
Am I doing something really wrong there

 

[dodobird]

Wit the reagents I have n all.. whats the easiest way to synth from 250 gms 2b4m using ea ma 40 and acetone and hcl38?

 

[dodobird]

Anyone?????

 

[dnBQByvHb8Zkawbjpx]

It looks like you have the process and all steps of the synthesis researched thoroughly. Here's my few notes:

• 500 ml acetone is too little for 250 g 2b4m. Have at least a liter, better 1.5 liters, available in your freezer. You may not need to use all but with 500 ml you would be rather short. Acetone used at this step can be recovered and reused again after a distillation.
• a magnetic stirrer/hot plate is an absolute must for consistency. It's the best $100 spent towards making 4-MMC .
• "drain ea ma layer which should be at the bottom" EA stays on top (it contains your free base), water that came from the MA aq 40 % is at the bottom. Drain water, like in all future washing steps.
• "does the flask need to be sealed or open here" always sealed, you can vent to release any pressure once done shaking
• your magnetic stirrer will not be able to work properly once the mixture thickens due to precipitated 4-MMC.HCl. Plan for this moment and have at least a spatula waiting, if not an overhead stirrer.
• dry acetone is acetone with as little water as possible. You should distill store-bought acetone to remove any contained water and impurities, but acetone purchased from trusted lab chemicals suppliers that is >99.5 % pure will work ok as well
• recrystallization does not require any other solvents than water, other solvents may speed up the process a little but they're costly so try and see how pure distilled water works for you. After some attempts with IPA and ethanol I don't use anything else anymore
• don't start with large (100 g or more) batches. Scale down the standard recipe to 1/4 and start with 25 g of BK4. That way you can confirm the process and everything works as you expect without wasting precious reagents before you get everything right. Once you confirm all is fine you scale up to 100 g batches or larger.

Hope this helps, good luck!

 

[Dr. MMX]

Other solvents are used depending on the need.
If product is pure - H2O is best choice.
If it was "more rought". IPA is excellent in the case.

 

[dodobird]

Thanks again mmx

 

[dodobird]

How big a glass container would I need for say 250mg 2b4m
Assuming no mag stir hotplate is available, would love some alternates and details ...maybe shake will work just once for a demo until further funds are released ?
Do I need to grind the 2b4m and any easy way to tell if the one I have is good enough
Will probably have a white crystalline powder rather thank the cream yellow I see many using, is that okay

How can I get to salt stage easily within 6 hours or 8?
Something between conventional method and shakebake and Voss to Ave tone and labware
Does every stage need glassware

 

[dnBQByvHb8Zkawbjpx]

For the reaction? Use whatever comfortably fits the required amount of solvent and methylamine. If you use 1000 ml EA and 500 ml MA then you should use a 2-liter flask/beaker.

There really isn't any alternative to a mag stir and a hot plate. Even a cheap one goes a long way towards consistency and repeatability. Vevor SH-2, new from official store, is €58 shipped, and may suffice already. SH-3 would be better and it's €103. I strongly recommend you consider getting a cheap hot plate + mag stir as only that will allow you to control temperature while stirring the mixture for hours at a consistent rate; and then repeat the same the next day without introducing unnecessary variability.

Grinding bk4 helps to dissolve it faster. Large clumps should be broken down, smaller ones will dissolve once you turn on stirring and preheat the RM to 20-30 °C which is a reasonable starting point for the reaction. The BK4 that I've seen contains both fine crystaline powder and some bigger chunks, it seems natural.

Easy, preheat the reagents to 30 °C in advance, dissolve BK4 in EA and stir until fully dissolved (my current BK4 has some insoluble contaminants, once all BK4 fully dissolves I filter the RM through a paper filter before I start the reaction). Then add MMA, once the temp starts to drop apply mild heat to keep the temp in 50-60 °C range and keep stirring until the reaction is complete. Then 3-4 rounds of wash with ice-cold distilled water to remove the excess MA and you have free base to acidify. It helps to put it in the freezer, once all is ready the acidification takes about 30 min if you add HCl really slowly (1 drop/s). That's when you have your salt ready to be filtered, this all can fit into 6-8 hours. But again, try it first with a smaller batch so you don't ruin valuable reagents with a simple mistake that can happen to rookie chemists.

 

[dodobird]

U da best!!

Please watch my messages or this thread to assist me over this weekend in case I get stuck at some stage, can't afford to not have a successful batch on this demo run, only then do I get to be in the money on the 20 and 100kg synths.
I know that is asking a lot from ANYONE but just in case you And other residents night find it in your heart to help this hard fighting old fart monetize knowledge to give my family an easier future that I know they deserve

 

[dnBQByvHb8Zkawbjpx]

I guessed based on your posts, no offense, we're all friends here.
Warm water will still work, but you may need to use more of it/do more washes to capture the same amount of methylamine that you would using cold water; and that will impact yield as more water will dissolve more EA and you'll lose some of the free base. If you can't get ice cold water which is strongly preferred then use warm, but understand the implications about lower yield.

 

[dodobird]

I didntvget the nonoffense n friend part bro..was supposed to say ..I'm only speculating the "like" at the beginning of the statement might not have been a good idea..Apologies for any mistake bro. Respect

 

[dodobird]

Wow thanks @dnBQByvHb8Zkawbjpx Just the kind of reply I was looking for, truly appreciated. Since the initial run is just like a test run might do 100g since another 20 kg awaits at hand. Once I find success with initial run I will surely be asking for the easy synth to scale it up in 2 0r 4 batches using non labware.
I don't truly know if mag stor is available with the person who I'm demoing to. Will heed ur word though. Do not want to carry any via domestic flight not even a mag stirrer I'll rough it out in a glass flask or bottle ...something like a voss method, knowing I will most likely need to heat up rm for nic layers.
Is the sod bicarb a must. WhT does it do and can I get same results using only warm distilled water during the wash of the freebase oil?
I'm curious at what stage does the gas need to be released ...read another post it us vital and dangerous if not released...guessing after ea affection. Pllease correct me

Thanks again. Pls pm me if u like always nice to see eager helpers like unselfish. Cheers

 

[dnBQByvHb8Zkawbjpx]

I'm happy to help, most of this is me passing the knowledge that I've learned from this forum, the local experts and my own experimentation. Your shared success story will be the best reward for my time.

A mag stir is such a basic equipment to any lab, that you should ask for it. Any professional will have it, only clowns will not.

The bicarb soda is not a must, some people use it, most probably don't. It is supposed to help clear up the free base from some shit. I think it's mostly used when methylamine hydrochloride was used in the reaction, it may be unnecessary when using aqueous methylamine.
For the wash you want to use ice cold distilled water, not warm! Your goal is to remove excess methylamine gas, and it dissolves best in cold water so that's what you need to use. Keep a bottle in the fridge, and put it in the freezer at the start of the reaction. By the time you need it it will be probably partially frozen and you can pour ice cold water.
I am not sure about the gas release, I've never had any considerable buildup that needed gassing out but others may correct me on this one.

 

[dodobird]

I saw some very helpful short videos in the forum as replies. Invaluable they are.

Anyone has any short videos to share from their aunty's for various stages of 4mmc synthesis??
Please share

 

[dnBQByvHb8Zkawbjpx]

See the video archive, there are several of them.

 

[dodobird]

Oops not aunty's but of their meph synthesis...lmao