Why hcl 30% not 35-38 % ?
4-MMC (mephedrone) synthesis in DCM
- Thread starter SonicNL
- Start date
no reflux condenser needed for this synthesis? Dcm heated to 40 degrees (boiling point) can sometimes lead to an explosion heated for such a time at such a temperature in a closed flask?
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- By TheVacuumGuy
It could be me, but read nowhere a closed flask was used. And why would you? Closed flask if pressure becomes too high the stopper will pop off nothing more nothing less
it's better praxis to use a condenser with a balloon or glove covering the exit, it's not necessary to stopper tight
I do this synthesis in DCM and use 0 heat, just good stirring and left overnight
I do this synthesis in DCM and use 0 heat, just good stirring and left overnight
probable rather than possible I would say, if the whole mass is at 40C in a closed glass system
the author's probably he's just SET it to 40C without measuring the temp of the mass or maybe I'm underestimating him
the author's probably he's just SET it to 40C without measuring the temp of the mass or maybe I'm underestimating him
If 40 percent methylamine solution is not available, can 15 percent be used? Would one just use 2.5 times more? For example if 200ml of 40% is needed, use 500ml of 15%.
Would the other reagents or solvents need an increase also? Or could those stay the same?
Would the other reagents or solvents need an increase also? Or could those stay the same?
the yield of said 4-MMC chemical synthesis route, with 30-45% do you mean the yield of mephedrone crystals after recrystalization?
Thank you!!
Thank you!!
It's possible he is not calculating yields by moles, with 24h reaction time in DCM at rt. yields are very good, above 40% for sure after crystalization
Hallo guys,
I also prefer method in DCM.
I mixed 100g of Bromketon in 300ml DCM and slowly added 200ml of Methylamin 40%a.q. solution.
Now my question, what temperature and what time would be the best.
Last time I kept temperature at 36 - 37 degrees and reaction-time was 3hours.
But the product was extremly blue after acification.
How can I repair the relation between temperature and cooking time best.
Smaller temperature = longer reaction time?
Which temperature are not working.
Can anybody help and explain the reasons of temperature and cooking time?
Thank you a lot.
I also prefer method in DCM.
I mixed 100g of Bromketon in 300ml DCM and slowly added 200ml of Methylamin 40%a.q. solution.
Now my question, what temperature and what time would be the best.
Last time I kept temperature at 36 - 37 degrees and reaction-time was 3hours.
But the product was extremly blue after acification.
How can I repair the relation between temperature and cooking time best.
Smaller temperature = longer reaction time?
Which temperature are not working.
Can anybody help and explain the reasons of temperature and cooking time?
Thank you a lot.
- By TheVacuumGuy
My experience is that you can easily do it at 40 (rm temp! Use glass thermometer which goes into your mixture). DCM seems very reluctant to start actually boiling (like it has some buffer zone of sorts). If I increase temp it stubbornly keeps sitting at 40.
Either way. That relation time/temp thing is only important for those in a constant hurry. The fact that a reaction takes a certain time doesn't mean you need to stopwatch tightly. Product doesn't walk away. On 35 overnight, 25 overnight, 40 in 2 hours, 40 in 8 hours . you'll get the same output (where, imho, longer = better).
Either way. That relation time/temp thing is only important for those in a constant hurry. The fact that a reaction takes a certain time doesn't mean you need to stopwatch tightly. Product doesn't walk away. On 35 overnight, 25 overnight, 40 in 2 hours, 40 in 8 hours . you'll get the same output (where, imho, longer = better).
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Thank you very much for your answer. I am just afraid, that, when I let everything react longer, that more side-products will increse and impury my product.
My last batch, I washed out the blue colour with acetone during filtering. I will send product to a labor to check, if it is good.
I also checked, that I used a little to much Methylamine. For 100g Bromketone I added 200ml Methylamine 40%a.q. solution.
I think 160ml should be enough (after calculation 1mol Bromketone vs. 2 moles Methylamine and a little buffer for Methylamine)
My last batch, I washed out the blue colour with acetone during filtering. I will send product to a labor to check, if it is good.
I also checked, that I used a little to much Methylamine. For 100g Bromketone I added 200ml Methylamine 40%a.q. solution.
I think 160ml should be enough (after calculation 1mol Bromketone vs. 2 moles Methylamine and a little buffer for Methylamine)
- By TheVacuumGuy
265,5.
The reaction I did shortly thereafter was one from 200g but used 800 dcm. This one yielded 165g. So that's around 75 percent (when accounted for some losses during crystallize). Much better than the one where used too little DCM.
So the 6 hour reaction I have to admit it didnt work as good (for future readers)
The reaction I did shortly thereafter was one from 200g but used 800 dcm. This one yielded 165g. So that's around 75 percent (when accounted for some losses during crystallize). Much better than the one where used too little DCM.
So the 6 hour reaction I have to admit it didnt work as good (for future readers)
How exacly did you worked for this? What is on last picture?
Reaction vessel is just standing in waterbath without stirring?
Reaction vessel is just standing in waterbath without stirring?