| Pages:
1
2 |
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
(M)ethyl alcohol will not form a separate layer with NaOH. IPA will not form peroxides not already present when distilled or evaporated in vacuo, and
I would think that peroxides in solvents would either decompose, not form, or react with other things when evaporated with many other cpds. besides
the solvent. BTW it is said that even ethers full of peroxides can be distilled to dryness uneventfully if the heat source is not too strong.
[Edited on 28-10-2019 by S.C. Wack]
|
|
|
Mush
National Hazard
Posts: 633
Registered: 27-12-2008
Member Is Offline
Mood: No Mood
|
|
May , but not in these reaction conditions.
NaBH4 would react with the peroxide as per this paper:
https://www.sciencedirect.com/science/article/abs/pii/S03603...
| Quote: |
but the crystals are dirty and don't clean up very well even with recrystallization -- this is why I would like to vacuum distill the freebase amine.
|
There are other ways to clean amines. Use one of this method.
You can also check the purity by tlc with 2 different solvent systems and stains. Compare the 2 against each other. If u get 1 single spot you are
good.
Shulgin distilled at 120-130 °C at 0.3 mm/Hg. If you are pro using such high vacuum then this is the way.
IMO distillation can be replaced with other purification methods.
[Edited on 28-10-2019 by Mush]
|
|
|
horribilis
Harmless
Posts: 30
Registered: 1-4-2019
Member Is Offline
|
|
Quote: Originally posted by Mush  |
May , but not in these reaction conditions.
NaBH4 would react with the peroxide as per this paper:
https://www.sciencedirect.com/science/article/abs/pii/S03603...
| Quote: |
but the crystals are dirty and don't clean up very well even with recrystallization -- this is why I would like to vacuum distill the freebase amine.
|
There are other ways to clean amines. Use one of this method.
You can also check the purity by tlc with 2 different solvent systems and stains. Compare the 2 against each other. If u get 1 single spot you are
good.
Shulgin distilled at 120-130 °C at 0.3 mm/Hg. If you are pro using such high vacuum then this is the way.
IMO distillation can be replaced with other purification methods.
[Edited on 28-10-2019 by Mush] |
I did not think of that -- it now seems obvious that that a >6 molar excess of NaBH4 would reduce peroxides. 
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
