Meow Meow "Voss" szintézis (4-MMC)

[animeboro]

brown mmc powder is created when we add the acid too quickly and the freebase starts to overheat, then all the pyrizine and other impurities start to come out, which means that we have lower efficiency. the same way we clean the wrong MMC free base, I use water and water with baking soda 3 times and water with baking soda always saves my life even when the entire solution did not react after rinsing with water and baking soda, I get the free base from the green oil of the MMC free base to yellow, changing the color green to blue and then to yellow

 

[William D.]

We can all rush, especially when the product is needed now But we can speed up the process of acidification with compulsory cooling, for example in a pan with cold water.

 

[mrchemist086]

@William D. can i make 3mmc using the same voss bottle method by using 3-methylpropiophenone and how to crystalize this please explain

 

[Come on 666]

1. Dissolve 2-bromo-4'-methylpropiophenone (100 g) and 400 mL of ethyl acetate in a "Voss" bottle.

2. Add 200 mL of 40% aqueous methylamine solution and shake the "Voss" bottle vigorously for 20 minutes. The mixture will heat up and change color. Do not keep the bottle cap tightly closed for a long time, otherwise it may explode. Open a small lid every 10-15 seconds for the first 5 minutes.

3. After 20 minutes, let the mixture stand until the layers are separated and the top layer is separated from the water, then rinse it once with cold purified water.

4. Dry the obtained free base with anhydrous magnesium sulfate and refrigerate it for 2 hours.

5. Add about 35-40 mL of 48% aqueous hydrobromic acid solution, add 1-3 drops and shake well. Adjust the pH value to between 5.5-6.

6. Put it in the refrigerator and freeze for 12 hours.

7. Add purified water in batches and shake until all the powder is dissolved. Then, we divided the powder into flat-bottomed heat-resistant glass containers and put them in the refrigerator.

8. After refrigerating in the refrigerator for 12 hours, we got a small needle-shaped crystal, but it was all over the mother liquor. We can filter it.

What I want to ask is:

1. Is this method okay for me? Is there any mistake that you can help me correct?

2. Do I need to control the temperature below 55℃ when adding methylamine? What effect does too high or too low temperature have on the product?

3. What effect will it have on the crystal if cold acetone is not used during crystallization? Will the color of the crystal become darker?