Please give it a read and help me
First i did 4mp -> 2b4mp
Chemical i used
4-methylpropiophenone
Hydrogen bromide 46-48%
Hydrogen peroxide 37%
Sodium bicarbonate
(I followed this synthesis - https://bbgate.com/threads/preparation-of-2b4mp-precursor-for-mephedrone.7042/ )
How i did it -
First i added 50ml 4mp to flask jar then added 40ml hydrobromic acid 48%, mix it, then slowly added 18 ml hydrogen peroxide 37% drop by drop while mixing the solution
Then i added cold water
And then filter the crystal
Then washed the crystal with soudim bicarbonate water and then dried the crystal
This is how it looked
Then i did 2b4mp -> 4mmc
This synthesis i followed - (https://bbgate.com/threads/the-simplest-recipe-for-crystal-mephedrone.7031/)
Chemical used -
2b4mp* - 50gg
Benzene - 100ml
Methylamine 40% - 70ml
Hydrochloric acid - 20ml
Chilled dry Acetone -
How i did it -
Added 100 ml benzene in flask then added 50g 2b4mp in the flask, mix it till it dissolved, then added slowly 70ml methylamine 40% to flask closed the lid of the flask and stirrir it using megnetic stirrer for 2 hour then after that i felt asleep after 6 hour again i stirrer it for 2 hour, then after that i stirrer it for 2 more hour, the mixture turned green by now, after that i gave mix it for on and off like every 2 hour i mix for 30 min till i completed 20 hour, mixture was still green
(I didn't use the heating method)
Then i pour the solution into the separating funnel and added 500 ml warm water and mix it then waited for separation then poured out the bottom layer, then repeat this process again
(It is mentioned in the synthesis that i should have a yellow colour solution but I had a greenish-bluish solution, why is that?)
Then i proceeded to the acidification step
I added free base 4mmc solution in the flask and then added chilled dry 200ml dry Acetone, mix it, then added hcl drop by drop to the solution, when i started the ph level was 9, but when i started adding acid its look like ph level was increasing (not sure check pick) after some time its look like ph level reached 3-4, so i didn't knew what to do so i reaserched and and i found out we can increase ph level of by adding soudim bicarbonate water solution to the mixture so i added around 30ml of this solution in mixture, it didn't work so i added more hcl drop by drop i added around 20ml of hcl and after that it somehow reached ph 5-6 i stopped the acidification and mix it for 10 more minutes
(The solution was still liquid it just changed colour green to red, when i added hcl, solution didn't become thick or something like that)
Then i pour out the solution and pack it in glassware and wrap it with plastic and put it in freezer, after 6 hour i took out the mixture and filter it thru paper filter, and nothing happened not a single drop of 4mmc powder was there
It feels so disheartening, after all this waiting and hard work, it didn't work, what do you guys think, what went wrong
I think maybe there could be 4 reason
1. After adding methylamine i should have heated it instead of waiting for 20 hour
2. I should have make the mixture of dry Acton and hcl and then added in the free base instead of mixing freebase with dry Acton then adding hcl
3. I shouldn't have added soudim bicarbonate water solution in acidification step
4. Maybe solution is too much, i should evaporate half of it and try again?
Please tell me what can i improve and what went wrong, and should i throw away the solution or can i still get 4mmc from that solution?
First i did 4mp -> 2b4mp
Chemical i used
4-methylpropiophenone
Hydrogen bromide 46-48%
Hydrogen peroxide 37%
Sodium bicarbonate
(I followed this synthesis - https://bbgate.com/threads/preparation-of-2b4mp-precursor-for-mephedrone.7042/ )
How i did it -
First i added 50ml 4mp to flask jar then added 40ml hydrobromic acid 48%, mix it, then slowly added 18 ml hydrogen peroxide 37% drop by drop while mixing the solution
Then i added cold water
And then filter the crystal
Then washed the crystal with soudim bicarbonate water and then dried the crystal
This is how it looked
Then i did 2b4mp -> 4mmc
This synthesis i followed - (https://bbgate.com/threads/the-simplest-recipe-for-crystal-mephedrone.7031/)
Chemical used -
2b4mp* - 50gg
Benzene - 100ml
Methylamine 40% - 70ml
Hydrochloric acid - 20ml
Chilled dry Acetone -
How i did it -
Added 100 ml benzene in flask then added 50g 2b4mp in the flask, mix it till it dissolved, then added slowly 70ml methylamine 40% to flask closed the lid of the flask and stirrir it using megnetic stirrer for 2 hour then after that i felt asleep after 6 hour again i stirrer it for 2 hour, then after that i stirrer it for 2 more hour, the mixture turned green by now, after that i gave mix it for on and off like every 2 hour i mix for 30 min till i completed 20 hour, mixture was still green
(I didn't use the heating method)
Then i pour the solution into the separating funnel and added 500 ml warm water and mix it then waited for separation then poured out the bottom layer, then repeat this process again
(It is mentioned in the synthesis that i should have a yellow colour solution but I had a greenish-bluish solution, why is that?)
Then i proceeded to the acidification step
I added free base 4mmc solution in the flask and then added chilled dry 200ml dry Acetone, mix it, then added hcl drop by drop to the solution, when i started the ph level was 9, but when i started adding acid its look like ph level was increasing (not sure check pick) after some time its look like ph level reached 3-4, so i didn't knew what to do so i reaserched and and i found out we can increase ph level of by adding soudim bicarbonate water solution to the mixture so i added around 30ml of this solution in mixture, it didn't work so i added more hcl drop by drop i added around 20ml of hcl and after that it somehow reached ph 5-6 i stopped the acidification and mix it for 10 more minutes
(The solution was still liquid it just changed colour green to red, when i added hcl, solution didn't become thick or something like that)
Then i pour out the solution and pack it in glassware and wrap it with plastic and put it in freezer, after 6 hour i took out the mixture and filter it thru paper filter, and nothing happened not a single drop of 4mmc powder was there
It feels so disheartening, after all this waiting and hard work, it didn't work, what do you guys think, what went wrong
I think maybe there could be 4 reason
1. After adding methylamine i should have heated it instead of waiting for 20 hour
2. I should have make the mixture of dry Acton and hcl and then added in the free base instead of mixing freebase with dry Acton then adding hcl
3. I shouldn't have added soudim bicarbonate water solution in acidification step
4. Maybe solution is too much, i should evaporate half of it and try again?
Please tell me what can i improve and what went wrong, and should i throw away the solution or can i still get 4mmc from that solution?
