The Hive > Methods Discourse

Bromosafrole-DMSO WTF???

<< < (4/4)

somniferous:
Yeah,
I've seen room temperature write-ups with aqueous Methylamine*HCl and write-ups using anhydrous methylamine. I've seen successes and failures with both methods. My decision to go one way versus another was arbitrary and based mostly on the lack (for now) of a workable "bomb". Even a 10% yield would be o.k. for now, as I'm just evaluating methods...

i.e.- Now that I've got a handle on the bromosafrole, I can figure out the best amination method at my leisure.  ;)

Gimme some sugar baby! -Ash, Army of Darkness

improv_chem:
I don't think you could do it that easily because the NH3 or MeAm would boil off with the heat. 
the amination can be done at room temperature with MeAm (so i've read) but will take a long time.  If you had iodosafrole it might be quicker.  mabe try swaping the Br for an I by heating the bromosafrole with some NaI in acetone for a while and then putting the iodosafrole in the MeAm/MeOH solution and stir for like a week or something??
sweet dreams;
--improv :)

--Preventing odors from escaping to nearby noses is essential.....

somniferous:
Hey,

From what I've seen on MW chem, people are using pyrex and leaving the lid a little loose so pressure won't build up. Since the glass is MW transparent, the top of the container remains cooler. Which might help condense the gas. I'm sure some methylamine would escape. But it's mixed at 10x molar, so there's a lot there. It's academic until I find a cheap, thrift store microwave to play with. (Not to mention a place to try, as I'm sure the reaction will stink to high heaven.) I'm really just wondering whether, under MW radiation, the correct reaction would even take place.

i.e.-It would really suck to do the reaction and make isosafrole.

If I get the chance to play I'll post results in the novel discourse. (With my luck :)  this will probably include at least a fire or two and maybe even an explosion. So it would be a good read.)

Instant X- You gotta admit, It'd be cool...

There's no business like the Devil's business! -Tibet 93

Osmium:
Using MeNH2*HCl will not work.
And heating substances to 100°C to dry them isn't recommended either, especially not with such delicate molecules as bromosafrole.

somniferous:
Thanks, I'd already surmised that the HCl salt wasn't going to work. I'm dreaming it with MeAm gas now...
I'll post the results.

As far as heating the 'Bromo'- I was only heating a small sample to see whether it'd break down at the same temp as my suspected 'di-bromo'.(It didn't.) Call it a sacrifice to the gods of chemistry... :( )
possible, as an unintended side rxn?


If so that would really suck. It would also explain some things...

Any ideas anyone?

Next dream I'm either keeping the everything cold for the whole 48 hours. That, or say "Fuck it!" and bubble the HBr into the DMSO...

There are three kinds of people - Those who can count and those who can't.

Navigation

[0] Message Index

[*] Previous page

Go to full version