Question Please look over my 4mmc recipe

[freedum]

Synthesis reagents:
100 g 4b4mp
300 ml DCM
200 ml of 40% MA solution.
1000ml 2000 ml reactor / FRBF
Magnetic stirrer 1000ML
Glass beaker 1000ml

Oxidation materials:
Distilled or deionized water 1000 ml
Hydrochloric acid ~35% - 30-40 ml
Buchner funnel
Separation funnel 1000 ml
Filtration flask 500 ml
Filtration paper 0.22
Negative pressure vaccum pump

Crystallization materials: (OPTIONAL)
IPA
Acetone
Shallow Pyrex dish
Glass spreader

Phase 1. (100g bk4 + 300ml DCM)
Dissolve 2b4mp in dichloromethane (DCM) in a reactor / flat bottom round flask.
(warm it slightly to help dilution 25ºC)

Phase 2 and 3 (200-ML of MA 40%)
Add a 40% aqueous solution of methylamine in batches so that the temperature does not rise above 40ºC. 50 ml every 5 minutes. ( total 30 min) DO NOT CROSS 40ºC

[methylamine addition causes exothermic reaction]

Phase 3 (do not cross 40ºC)
Keep mixing solution for 4 hrs at ~35ºC.
Turn on the heat as soon as the temperature begins to drop.
AFTER 4 hours transfer to glass beaker.

GLASS BEAKER on stirrer
Phase 4.
FIRST WASH: Add 500 ml 5% sodium bicarbonate solution around 30ºC
(Separate the layers as much as possible with overhead stirrer)

TRANSFER to Separation funnel.
let sit 60 min (drain bottom layer)

GLASS BEAKER / stirrer / mixer
2nd wash 200 ml demi water at 30ºC
Stir well for about 10 minutes.
Transfer to separation funnel

SEPERATION FUNNEL.
Let sit 4MMC solution sit for 30 min
If a bit cloudy add a dash of sodium bicarbonate shake in separation funnel and let sit for 30 minutes. Drain bottom water layer. Transfer to Glass Beaker.

GLASS BEAKER
Phase 5 (150ml Acetone + 30ml HCL)
Add ICE COLD acidification mixture drip by drip into it 4mmc solution while magnetic stirrer is on a high setting. Keep checking ph levels. When PH level reach 5 stop and transfer to a plastic beaker. Set in fridge for 10 hours.

( you do not have use all your solution, only the PH level is important)

GLASS BEAKER small ( quality check)
Phase 6.
Grind 4mmc solid to powder
Take 1 gram of powder and disolve in demi water at 90 ºC
Now we can see the solution colour.
The darker the colour the more impurities are present. We want to see a clear solution. If not clear we need extra purification. ( atleast darker than the colour of a lemon)

Vaccum filter.
BUCHNER FUNNEL / Glass spatula
Phase 7. (Ice cold acetone)
Place crushed powder into funnel and first use a small bit of cold IPA, after that wash in acetone all while gently stirring the 4mmc on the filter paper. Allow the IPA and Acetone to evaporate before applyimg more so the 4mmc dosent Dissolve into the alcohol.
Make sure the powder is more of a free moving thick liquid consistency. If it is clay like it can clog the filter paper.
Leave the vaccum running for a bit untill you have a dry consistency.
Transfer the powder to a dish and use a infrared light to finish the drying, in a warm dry room.
It's ready when it has a powdery refractive look.
DO NOT THROW WASTE LIQUID

YIELD.
If your overall weight has lost a large % of mass its possible 4MMC is still in the IPA and acetone. Allow more than 50% of the liquid to evaporate slowly, and run it through. The filter again

CRYSTALLISATION (optional)

GLASS BEAKER / heated mixer.
(1g to 1ml Demi water/1ml IPA)
Mix your 4mmc into your solution heat to around 80ºC (very small bubbles) all while running your magnetic mixer vigorously.

CRYSTALLISATION DISH
(Pyrex can take heat and cold)
phase 9.
Pour the 4 mmc solution into dish
Preferably leave to crystallize in a dry room at 18-20ºC. It is preferable to use an air conditioner. When crystallization stops put into the freezer for 8 hours
The more water you use, the larger the crystals and the longer it will take once done remove crystals from dish
Wash crystals with ice cold acetone in Buchner funnel, once or twice.

 

[Osmosis Vanderwaal]

Well you should delete the copy in synthesis, as it is more for proven methods. You never add more cleaner (water) than solvent, so no to 500ml of nahco² water to 400 ml solvent precursor. There were a couple of other no no's I saw. I didn't balance any reactions.
So, there's this long standing rarely mentioned rule. It's called, if you haven't done it before [bold]FOLLOW THE TEK[/BOLD]
It's easy to do, you just read what someone who knows what they are doing wrote, then you try to do the exact same thing.
It doesn't hurt to read several techniques, but when it is time to start, PICK ONE AND STICK WITH IT. Don't mix and match parts of several, you'll fuck it up. I understand the desire to innovate, but you can't possibly innovate until you know the history of what's been done. There's very few examples in history where a noob innovated anything. Of those 0 were chemistry. Good luck.

 

[freedum]

Not innovating. This is mostly 1 method posted by sonic. I added bits of extra insight and expanded on certain areas to add clarity. Please stipulate the area that need changing greatly appreciated brother. As I said I will. Record it all to contribute to the community and I'll give away a bunch to members to spread the knowledge.

 

[Osmosis Vanderwaal]

There's a formula for cleaning product with an immiscible solvent. It involves the solubility of the substance in each solvent it works out to 50% as much 2 or 3 times, or 50%, 30%. It's never 100% or more. If you want to post something useful do the math. Show the math. Explain the math. Explain the reaction mechanism. Talk about the bond kenetics. Add something more than," stir the mixture as slowly as possible, as to not form an emulsion" By the time you do the math you will have learned a lot more than clearing up some ambiguous language.

 

[freedum]

And exactly this is the issue. You assume I know what your going on about.. speaking without actually helping, to my understanding this is a place to learn. Or am I mistaken about this?

Your going on about the formula, what formul? Your referring to the IPA and demi water ?
How about you jump off that horse and you try to explain the science behind it. Your acting like you were born with this knowledge. You claim to know so much about it yet never actually clarify anything or add anything useful. One of us is on the wrong forum. If this is not a place to share knowledge and discuss stuff let me know.

 

[Osmosis Vanderwaal]

There's an unspoken rule, that we often speak about. It's the broadly accepted theory that by " holding your hand" and giving you the answers without you making the effort to find the answer yourself, that you will be Ill prepared to accomplish these chemistry goals safely.
Your response exemplifies what I mean. Somehow you became upset that I suggested you learn any chemistry and demanded easy answer to your questions having made no effort. It's quite an entitled position, that of a spoiled 12 year old girl perhaps.
Of course I wasn't born with any chemistry knowledge. No one hand fed it to me either. Years of research has gotten me what knowledge I have. There's a special reaction taking place in this synthesis and it only works with a certain kind of chemical. It's the alpha keto halogenation. It installs a halogen on the alpha carbon of a ketone. This is a really great thing. If a person could do the same to an alkylamine, meth you be a 1 pot 2 step reaction. The difference between ephedrine and meth is a methyl moiety on the alpha carbon. To understand the kenetics of this reaction Read this wiki entry.
For the liquid -liquid clean up you blindly throw numbers at, you should understand it a lot better after you have learned about Liquid liquid extraction kenetics.
If you are too lazy to do that, don't waste your time writing garbage nonsense about something you know nothing about and spend that time looking for renters insurance for when you burn your Mom's house trailer down, which you will do.

 

[freedum]

Cool story bro. FYI any figures I've out here come from the people who run this site. Knowledge I believe should be easily spread. You could have taken two approaches here. One being a massive cocktail, or two sent links to text, maybe videos of examples of similar reactions maybe on YouTube, or maybe even write a small paragraph outlining a few stuff with some sort of , this is called x and you can read more about it here. Which. I am very interested in learning what this section of the synthesis is called, and I am very much interested in knowing the fundamentals so o cab apply it to any type of chemistry.

You however choose to once again. Display your superiority to someone who came here woty zero knowledge, spent a few hours going through various posh and is trying to build a better understanding with almost no help. You say if you don't know follow the synthesis posted to the letter. Then you say I should do calculations and then you provide nothing. Best of luck to you mate

 

[Osmosis Vanderwaal]

Wut the fuck bro? You don't speak English? I told you what it's called, I linked you to 1500 words on the synth I linked you to the exact math. The correct next move for you is to read it. Look up the words you don't know. Then you come back and ask specific questions about what you don't understand. Did you look up what makes something a ketone? You know I give a fuck less but people ain't going to want to help you with that entitled attitude and lack of desire to help your self. You can't learn this by being told. I could tell you how to lay a brick, or finish concrete or paint a house, but you won't be any good at it until you get in there and learn for yourself.

 

[freedum]

You don't want to eat me. Wait for my brother he's much fatter than me.

 

[Albert]