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For me the trick to not get sludge for cas 5449-12-7 was to dissolve in boiling water to a clear solution, turning off heat and carefully adding h2so4 conc.
This got me instant conversion in acceptable yield, with layers forming immediately, but I still refluxed 30 min to be sure.In contrast when I hurried and did not dissolve my glycidate completly no amount of reflux was able to get the solids to react and had to filter them.
Careful of the splashing when adding acid.
This got me instant conversion in acceptable yield, with layers forming immediately, but I still refluxed 30 min to be sure.In contrast when I hurried and did not dissolve my glycidate completly no amount of reflux was able to get the solids to react and had to filter them.
Careful of the splashing when adding acid.
- Joined
- Apr 29, 2023
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- 89
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- 1
- Reaction score
- 48
- Points
- 18
For me the trick to not get sludge for cas 5449-12-7 was to dissolve in boiling water to a clear solution, turning off heat and carefully adding h2so4 conc.
This got me instant conversion in acceptable yield, with layers forming immediately, but I still refluxed 30 min to be sure.In contrast when I hurried and did not dissolve my glycidate completly no amount of reflux was able to get the solids to react and had to filter them.
Careful of the splashing when adding acid.
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OrtistU think so? Separated from what? And what is left if it separated?
BMK has a pretty light aroma, have u compared with smell after reflux?
I'm not saying you don't know how it smells or that I am not wrong, just looking to know
UWe9o12jkied91dSeparated from sodium . Actually I am struggling now with 5449. Tried bunch of methods and so far got 1ml from 10g. Will try phosphoric acid at 110. When I add acid to 5449 it turns to oil very quickly but it is not p2p. Or may be my 5449 is not real 5449
OrtistFair enough, it may be so.
I can speak for large scale and with 2-3 hour reflux this time but phosphoric and citric both work great. For citric 25kg/20kg 5449.
UWe9o12jkied91dHave you tried phosphoric route? Do I need to add dry powder straight to hot acid with stirring or powder has to be dissolved in water prior to addition?
OrtistHad ok results with dissolving both in minimal amount of water as well as 1L water/kg. Both ways made warm and followed by acid and refluxed.
Cant tell u how much is minimal compared to 1L/kg.
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With H2SO4 layers separate instantly but that doesn't mean you got P2P. It is just glycidic acid separated. I just stried it and got two layers with no smell.
BMK has a pretty light aroma, have u compared with smell after reflux?
I'm not saying you don't know how it smells or that I am not wrong, just looking to know
- Joined
- Apr 29, 2023
- Messages
- 89
- Solutions
- 1
- Reaction score
- 48
- Points
- 18
U think so? Separated from what? And what is left if it separated?
BMK has a pretty light aroma, have u compared with smell after reflux?
I'm not saying you don't know how it smells or that I am not wrong, just looking to know
- Joined
- Aug 8, 2022
- Messages
- 679
- Reaction score
- 501
- Points
- 63
- Deals
- 5
Separated from sodium . Actually I am struggling now with 5449. Tried bunch of methods and so far got 1ml from 10g. Will try phosphoric acid at 110. When I add acid to 5449 it turns to oil very quickly but it is not p2p. Or may be my 5449 is not real 5449
I can speak for large scale and with 2-3 hour reflux this time but phosphoric and citric both work great. For citric 25kg/20kg 5449.
- Joined
- Apr 29, 2023
- Messages
- 89
- Solutions
- 1
- Reaction score
- 48
- Points
- 18
Fair enough, it may be so.
I can speak for large scale and with 2-3 hour reflux this time but phosphoric and citric both work great. For citric 25kg/20kg 5449.
- Joined
- Aug 8, 2022
- Messages
- 679
- Reaction score
- 501
- Points
- 63
- Deals
- 5
Have you tried phosphoric route? Do I need to add dry powder straight to hot acid with stirring or powder has to be dissolved in water prior to addition?
Cant tell u how much is minimal compared to 1L/kg.