Is it possible to add hydrobromic acid to ethyl acetate without using acetone?

[Come on 666]

This is my experiment today

1. Pour 100g of dry BK (bromoketone; 2-bromo-4'-methylphenylpropiophenone).

2. Pour n-methylpyrrolidone (400mL) into the reactor. Start the overhead stirrer and heat the reaction mixture to 33°С. (The weather temperature is high so no heating) Stir the reaction until BK is completely dissolved in NMP.

3. Pour all 40% methylamine aqueous solution (200 mL) into the reactor, because the reaction material is still a little short of touching the thermometer, the thermometer shows 50℃. React for 20 minutes.

4. Next, pour 1 L of distilled water at 4℃ into the reaction mixture and stir for 2 minutes.

5. Pour 500mL of ethyl acetate into the reactor and stir the mixture for 2 minutes.

6. Then, stop the stirrer and the mixture separates into two layers. Wash twice with 500mL of cold distilled water.

7. Pour the upper alkaline extract containing EA into a beaker, dry it with anhydrous magnesium sulfate, and store it in a refrigerator at 4°C.

8. Turn on the stirrer and slowly add 500mL of cold acetone to the reaction mixture, and add 48% hydrobromic acid dropwise under constant stirring until the pH value reaches 5.5-6.

The liquid turns black and no crystals are seen. No crystals appear after refrigeration. Later, I poured out all the liquid. What caused this?

Can I add hydrobromic acid directly to the mephedrone free base in ethyl acetate?

Are there any consequences for not using acetone for crystallization?

 

[mephedrone_4-mmc]

The liquid turns black and no crystals are seen. No crystals appear after refrigeration. Later, I poured out all the liquid. What caused this?


Same error

 

[mephedrone_4-mmc]

You find any solution for that .

 

[prvnc]

Adding hydrobromic acid directly to the free base in ethyl acetate may cause solubility issues, preventing crystal formation. Acetone helps by changing solvent polarity and promoting crystallization. Without it, the acid might not precipitate the salt efficiently, leading to a black solution with no crystals. For best results, follow the original procedure using acetone or try alternative solvents with similar polarity. Skipping acetone likely disrupts salt crystallization, affecting purity and yield.

 

[fancypants]

So it is possible to acidify by adding water to the EA with 4-MMC freebase solution?

If yes, what would be the water to solution ratio?

 

[Come on 666]

So I still have to use -10℃ acetone to crystallize as shown in the video, right?

 

[Come on 666]

But I also used cold acetone in the experiment. Why did the liquid still turn black and no crystals were seen?

 

[Come on 666]

I synthesized 2-bromo-4'-methylpropiophenone according to the method in the video，

However, the synthesis of 4-MMC using 2-bromo-4'-methylpropiophenone failed.

And I don't know where the problem is,Is there anyone who has successfully synthesized 4-MMC? Please help me, we can discuss the synthesis of 4-MMC together.

 

[mephedrone_4-mmc]

4mpp to 2b4m.
Then 2b4m to 4mmc.


4mpp.
Hbr
H2o2

Your get 2b4m liquid

Liquid 2b4m.
EA.
MA 40%


WASH WITH 10% NAOH OR BAKING SODA with 1 TIMES.
Then cold water wash with 4 times.

THEN COOL IT SOLUTION -15DEGREE FOR 12 HOURS

IN SOLUTION ADD -15 DEGREE ACETONE.
STIRRER 10 TO 15 MIN.

5 KG SOLUTION 10 KG ACETONE
I USED WEIGHT MACHINE.

THEN START ADDING HBR FOR ACIDITY. Until PH 5.

After that OPEN THE LID AND blow air.

I USED DC FAN FOR BLOW ALL AIR AMD SOLUTION.


STIRRER AND BLOW AIR FOR ALL ACETONE DISAPPEARED.

ITS NORMALLY TAKES 12 HOURS.
IN THAT TIME SOME SAME PARTICAL form BUT ITS NOT CRYSTAL ITS ONLY POWDER.

Wash with acetone

WHAS IT HEAT WITH SOME SOLUTION THEN YOU GET CRYSTAL.

 

[Come on 666]

Why should you clean once with 10% NAOH or baking soda?Because they say that this will cause the ethyl acetate to decompose and be difficult to separate from the water.What is the purpose of cleaning?

Thank you for your reply. I will continue to experiment according to your method and leave a message here later.

 

[mephedrone_4-mmc]

For washing freebase solution.
If we directly do acidification solution turn in red. And other impurities left.


So wash stirrer 5 min. Then add in seperate funnel.
20 min left both layer form.

After final wash solution color look like yellow.

When we perform acidification the solution becomes hot due to exothermic reaction, however cooling the solution and acetone gives good result, sometimes if I have to do it like that after acidification I got the powder so I stayed for 12 hours,

For good quality product washing is good

 

[Come on 666]

100 g 2-bromo-4'-methylpropiophenone，N-Methyl-2-pyrrolidone (NMP; cas 872-50-4) 400ML，Methylamine 40% aqueous solution (cas 74-89-5) 200 ml，Ethyl acetate 500 ml
What concentration of sodium bicarbonate in water should I use for cleaning?
How many milliliters of sodium bicarbonate solution should I use?

 

[mephedrone_4-mmc]

Simple i heat this black 2 layer solution at 50 degree.
Then pour bottom layer in tray temp at 46 degree.
Top layer discard.

And slowly decrease temp 2 degree in 30 min. Time lapse. With hot air.
Not crystal for but i found dark red colour layer thick solution.
Its take 3 house total.
Then off the heat temp.
After that put tray in full speed fan for 5 hours.

Fully dry and solid layer.
I used 1 litter acetone for 300g gram product.

In 2 litter beaker add 1 litter acetone then add 300gram product and gently stirrer 10 min
All dark colour dissolved in acetone.

Filter the product using vaccum filter.
Product look like reddish yellow.

I have product above 50kg
Next step after that

 

[mephedrone_4-mmc]

If you think who I'm.
Google it

nagpur md drug, opretion thunder..

 

[mephedrone_4-mmc]

For washing freebase solution.

If we directly do acidification solution turn in red. And other impurities left.





So wash stirrer 5 min. Then add in seperate funnel.

20 min left both layer form.



After final wash solution color look like yellow.



When we perform acidification the solution becomes hot due to exothermic reaction, however cooling the solution and acetone gives good result, sometimes if I have to do it like that after acidification I got the powder so I stayed for 12 hours,



For good quality product washing is good

 

[Come on 666]

Is it necessary to use cold sodium bicarbonate solution when cleaning with sodium bicarbonate solution?

 

[Come on 666]

A 5% sodium bicarbonate solution was added, and the mixture was stirred for 5 minutes. Ethyl acetate was then added, and the mixture was stirred for 5 minutes.
Add 5% sodium bicarbonate solution and continue to add ethyl acetate and stir for 5 minutes.
How do I operate

 

[Come on 666]

Anhydrous magnesium sulfate is not used in any of the videos. Why is that?Is it not necessary to dry the free base in ethyl acetate before crystallization?

No, anhydrous magnesium sulfate (MgSO4) is not suitable for drying free alkali. While it's a common drying agent for organic solvents due to its affinity for water, it will react with and be consumed by strong bases like free alkali. The reaction will neutralize the alkali and produce magnesium hydroxide and magnesium salts, rendering the MgSO4 ineffective as a drying agent and potentially contaminating the material you are trying to dry.

Is this statement correct?

 

[mephedrone_4-mmc]

No use

 

[Come on 666]

So do I need to dry the free base with anhydrous magnesium sulfate?

 

[mephedrone_4-mmc]

No. Where you read about magnesium sulfate.

 

[Come on 666]

Mephedrone synthesis (4-MMC) in NMP solvent. Large scale.

Reaction scheme: Reagents: 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) - 5 kg; n-Methyl-2-pyrrolidone (NMP; cas 872-50-4) - 20 L; Methyl amine 40% aq. solution (cas 74-89-5) - 8 L; Benzene - 20 L; Acetone - 30 L; Hydrochloric acid con. aq. solution (HCl 36%) ~ 1.5 L; Distilled water - 20...

bbgate.com

4-MMC (mephedrone) synthesis. Bromination in dichlormethane.

We'll consider mephedrone (4MMC) synthesis in this article. Dichloromethane (DCM) is used as a solvent. It has a low boiling point (~40 °C) and synthesis procedures take a little time. Work conditions: Air temperature 20-24 ºC; Relative humidity

bbgate.com

Both articles say to use anhydrous magnesium sulfate for drying, but other videos and articles do not use anhydrous magnesium sulfate.

 

[Come on 666]

I bought hydrochloric acid. It will arrive in a few days, and I will do the next experiment, because I think hydrobromic acid is not very good. I want to use hydrochloric acid, and I will report the results to you when the time comes.

 

[mephedrone_4-mmc]

I used hydrobromic acid for acidification