- Joined
- Oct 15, 2022
- Messages
- 32
- Reaction score
- 15
- Points
- 8
Just wanna add an update on a similar synthesis.
I mixed,
142 benzaldehyde
100ml nitroethane
7ml n-butylamine
And mixed at room temperature for 6 hours.
Observed a nice orange color so added 100ml of IPA and put in the freezer over night.
I awoke to an ice cold mixture of 0 crystals.
So not 1 to give up I removed RM from freezer and place in a rb flask on a water bath and added a reflux condenser.
When it started refluxing not sure on exact temp but about 80 degrees celcius I added 25ml of Gaa and continued for 4 hours.
After reflux I placed straight into freezer to awake to a solid mass of dirty crystals
Filtered them on a buchner with vacuum and wased with cold IPA.
put 100ml of IPA in a beaker and added all washed crystals and heated until all had dissolved at about 70-80 degrees celcius and placed back in freezer.
Within minutes I'm getting needle like crystals forming will post total weight after fully getting down to temperature and re filtering and drying.
Just wanted to add this to tell people not to give up on RM if you don't get crystals 1st time. I will add a pick of crystals formed so far!
I mixed,
142 benzaldehyde
100ml nitroethane
7ml n-butylamine
And mixed at room temperature for 6 hours.
Observed a nice orange color so added 100ml of IPA and put in the freezer over night.
I awoke to an ice cold mixture of 0 crystals.
So not 1 to give up I removed RM from freezer and place in a rb flask on a water bath and added a reflux condenser.
When it started refluxing not sure on exact temp but about 80 degrees celcius I added 25ml of Gaa and continued for 4 hours.
After reflux I placed straight into freezer to awake to a solid mass of dirty crystals
Filtered them on a buchner with vacuum and wased with cold IPA.
put 100ml of IPA in a beaker and added all washed crystals and heated until all had dissolved at about 70-80 degrees celcius and placed back in freezer.
Within minutes I'm getting needle like crystals forming will post total weight after fully getting down to temperature and re filtering and drying.
Just wanted to add this to tell people not to give up on RM if you don't get crystals 1st time. I will add a pick of crystals formed so far!