Hello again to the experts, friends and all chemists
I have posted a threat about my problem with the yield which it was not more than my finger tip size, and some nice guys gave me some advice and tips, and I considered them.
So this young chemist repeated the synthesis with his broken hand
and got to the same issue, but enjoyed sharing more details for you comrades hope to solve the riddle
.
.
My scale was
-25g propiophenone
-50 ml of a diluted Hbr (that i had made it via 20g KBr in about 70-80ml Distilled water, adding 15ml H2SO4 dropwise, freezed the solution to divide the side-products, then heated to evaporate then got the distilled solution contain Hbr.)
-15ml H2O2 35%
-75ml DCM
-12g Na2CO3 in 250ml DW(distilled water)
-35ml Methylamine 40% aqueous solution
-25ml HCl 14% solution (I got that from diluting 10ml HCl 38% in 15ml DW)
-another 10ml DCM and 20ml Water contains 0.5ml HCl
Now the process:
1. Adding propio to the flask, adding Hbr solution, then adding H2O2 dropwise in about 40min while the solution was being stirred in room temperature
2,3. Adding DCM, and washing it to neutralized(for washing i transfer the reaction mixture into the decanter, after that i pour it back into the flask.)
4. Adding Na2CO3 solution divided in 2 portions(2x125ml), then washing it to neutralized.
5. I add all the methylamine at once, put the reflux condenser, and stir it for 1.5h in room temperature.
5.5 I washed it 3-4 times with about 75ml DW, it was still alkaline then.
6. I added Hcl solution (i did it too fast so a lot of fog occured in the flask, next time I will handle that), stirred for 1 hour in room temperature.
7. I take out the dcm layer, wash it with that acidified DW i had said before. Then i mixed first and this aqueous layer and washed them with 10ml DCM.
8I poured the solution into a beaker and heated it until crystallization.
9. Finally this is what i’ve got
___________________
I need to figure my mistake
What did i forget?
Where was i wrong?
Please notify me!
.
Great love to all…
I have posted a threat about my problem with the yield which it was not more than my finger tip size, and some nice guys gave me some advice and tips, and I considered them.
So this young chemist repeated the synthesis with his broken hand
and got to the same issue, but enjoyed sharing more details for you comrades hope to solve the riddle.
.
My scale was
-25g propiophenone
-50 ml of a diluted Hbr (that i had made it via 20g KBr in about 70-80ml Distilled water, adding 15ml H2SO4 dropwise, freezed the solution to divide the side-products, then heated to evaporate then got the distilled solution contain Hbr.)
-15ml H2O2 35%
-75ml DCM
-12g Na2CO3 in 250ml DW(distilled water)
-35ml Methylamine 40% aqueous solution
-25ml HCl 14% solution (I got that from diluting 10ml HCl 38% in 15ml DW)
-another 10ml DCM and 20ml Water contains 0.5ml HCl
Now the process:
1. Adding propio to the flask, adding Hbr solution, then adding H2O2 dropwise in about 40min while the solution was being stirred in room temperature
2,3. Adding DCM, and washing it to neutralized(for washing i transfer the reaction mixture into the decanter, after that i pour it back into the flask.)
4. Adding Na2CO3 solution divided in 2 portions(2x125ml), then washing it to neutralized.
5. I add all the methylamine at once, put the reflux condenser, and stir it for 1.5h in room temperature.
5.5 I washed it 3-4 times with about 75ml DW, it was still alkaline then.
6. I added Hcl solution (i did it too fast so a lot of fog occured in the flask, next time I will handle that), stirred for 1 hour in room temperature.
7. I take out the dcm layer, wash it with that acidified DW i had said before. Then i mixed first and this aqueous layer and washed them with 10ml DCM.
8I poured the solution into a beaker and heated it until crystallization.
9. Finally this is what i’ve got
___________________
I need to figure my mistake
What did i forget?
Where was i wrong?
Please notify me!
.
Great love to all…