Distillation of Safrole

[rickcha37]

please help when heating the sassy  with a simple distillation getting exlpodeing bubbles that are going up and over all the way to collection the heating process is stirring as well as heating. any idea s

[Stonium]

Strong stirring.

[wyndowlicker]

Hey now,



How about your temp?

[methyl_ethyl]

Ideas, yes, how many mL's of Sassy do you have in your boiling flask, and what is the capacity of your boiling flask?

ie. 1000mL of sassy in a 1000mL boiling flask = not a good idea.

     More information please.....

[technology]

As mentioned Make sure you are using good stirring and, never fill the flask more than half full, and also lower the flask with your oil into the heating oil so that it is below the line of the oil you are heating to heat the oil (fuck i almost lost my self in that explanation) also you can put a stir bar in the oil you are heating to heat the sassy which will also evenly distribute the heat also.

check this out

http://www.chem.cuhk.edu.hk/labtech/index.asp

very good clips of distillation, vacuum etc

Also you said simple distillation are you using vacuum, you can get away without vacuum of the top f my head, but i am sure all recommend vaccum, i do!

[abolt]

Post 292562

(wyndowlicker: "cant get safrole? FREEZE IT!", Methods Discourse)

[slick14]

Swim has also encountered the exploding bubbles and has found that gradual heating will stop them. Good Luck

[technology]

yes another good point there,

always heat slowly, though some have mentioned heating it fast to the desired temp. It all depends on the time you have. slow is better!

[nitrous351]

All of the previously mentioned ideas work the best for preventing bumping (the phenomenon described in the original post), but an added safeguard would be to plug the bottom of your distillation adapter with glass wool. When I say "plug" I don't mean "stopper." Just have a piece of glass wool inside the tube just tight enough so that it won't fall out.
If you have plenty of cheese, you can order a fritted distillation adapter. A fritted distillation adapter has a built-in glass frit. It looks like the perforated part of a buchner funnel inside your adapter. Hope this helped. peace

[aleph]

If stirring isn't available, try using boiling stones.  Also, distill at a reasonable rate; don't try to get it done in a hurry.  Patience is a virtue.

[mindlib]

As far as I know, it´s better to use a vigreux-column and a special apparatus between the "dest-column" and the receiving flask. Look Laptop. I think, you will anyway "need" it later, when you destill other products of your synthesis plan.
The vigreux column should be short (200-300 mm).
advantages: better seperation, more effective, less time using da apparatus Laptop told.

[mindlib]

"but i am sure all recommend vaccum, i do!"
I do,too!