First of all, I use benzene 1 L to dissolve 500g of 2b4m, and it can’t dissolve completely at the beginning, so I heat it up a little until it dissolves, after that, the solution is warm but not boiling. I used 10L round bottom flask
2. I prepare the NaOH aq solution (300g of NaOH and 600ml water, just enough to dissolve it), I let it cool to room temperature, then I add it to the part 1 solution. Right after I add it at once, some deep brown oil coming up, then I start the stirring, the whole thing turns to brown and release some smoke ( just little), then I measure the temperature immediately, it is around 40-45 degrees. And I never stop the stirring.
3. I prepare 400g of MA.HCI, I added it in very small portions, around 10-20g each time, it took me around 2 hours to finish, because I keep the temperature around 45. And I can see the bottom has NaCI keeps piling up, and has some bubbles coming from bottom too. After I added all the MA.HCI, I keep stirring until it temperature drops itself.
4. I filter the NaCI out, and I wash it with water Twice, the whole solvent is still dark, then I proceed to acidification with 5:1 acetone and HCI until ph5, drop wise with needle. But still dark.
I afraid I was done something wrong, in fact, as long as I texting this reply, that dark solution is currently sit in my fridge for 3-4 hours already. I’m really seeking help about it, I pray I could have some result tomorrow, best regards.
2. I prepare the NaOH aq solution (300g of NaOH and 600ml water, just enough to dissolve it), I let it cool to room temperature, then I add it to the part 1 solution. Right after I add it at once, some deep brown oil coming up, then I start the stirring, the whole thing turns to brown and release some smoke ( just little), then I measure the temperature immediately, it is around 40-45 degrees. And I never stop the stirring.
3. I prepare 400g of MA.HCI, I added it in very small portions, around 10-20g each time, it took me around 2 hours to finish, because I keep the temperature around 45. And I can see the bottom has NaCI keeps piling up, and has some bubbles coming from bottom too. After I added all the MA.HCI, I keep stirring until it temperature drops itself.
4. I filter the NaCI out, and I wash it with water Twice, the whole solvent is still dark, then I proceed to acidification with 5:1 acetone and HCI until ph5, drop wise with needle. But still dark.
I afraid I was done something wrong, in fact, as long as I texting this reply, that dark solution is currently sit in my fridge for 3-4 hours already. I’m really seeking help about it, I pray I could have some result tomorrow, best regards.
- By Dr. MMX
1st put that into freezer for 12h, maybe you will get something out of it 
Why use benzene? cant get other solvents?
why that proportions. Did you read before adding it or what was the rason of such amounts 200 ml solvent 100g 2b4m, and methylamine in suchproportions. Why?
I can only guess, but probably 2b4m wasnt fully dissolvedor temp was already too high. Never happened to me to turn out dark in the start. There canbe other factors as well. Temperature was high there could be some reaction with benzene and NaOH.
For future, if youwanna to change soemthing just 1st check, it will avoidmistakes.
I suggest you just simply go for ethyl acetate and just keep the proportions ok?
now just as isaid in the start, put into freezer for 12ha nd go filtration aftert that, maybe youwill receive some of product, youcanshowme later what you have.
Why use benzene? cant get other solvents?
why that proportions. Did you read before adding it or what was the rason of such amounts 200 ml solvent 100g 2b4m, and methylamine in suchproportions. Why?
I can only guess, but probably 2b4m wasnt fully dissolvedor temp was already too high. Never happened to me to turn out dark in the start. There canbe other factors as well. Temperature was high there could be some reaction with benzene and NaOH.
For future, if youwanna to change soemthing just 1st check, it will avoidmistakes.
I suggest you just simply go for ethyl acetate and just keep the proportions ok?
now just as isaid in the start, put into freezer for 12ha nd go filtration aftert that, maybe youwill receive some of product, youcanshowme later what you have.
- By WalterFan
I used benzene is because I saw another synthesis can apply it as solvent, and ethyl acetate is ban in my city; about the ratio of methylamine is because I watched another article about 1 mole of 2b4m combine 1 mole of methylamine can form 1 mole of 4-mmc, but what I have is MA.HCI, so 400g of MA.HCI is contained 200g around MA, in considering my poor cooling condition, so i decided to use 2 times amount of methylamine for 500g 2b4m.
im really thankful for your reply, I get back to you later, I hope I can get something out of it too
im really thankful for your reply, I get back to you later, I hope I can get something out of it too
- By Dr. MMX
Use more solvent next time, it will be easier to maintain temperature, and check it whats actual temp to control its situation. You can use water bath as well.
probably you will get a lot of impurities, so 1st make it dry then use acetone with slowly fitlration, maybe you will still get something out
probably you will get a lot of impurities, so 1st make it dry then use acetone with slowly fitlration, maybe you will still get something out
