posted 12-05-1999 09:14 AM         

My basement is like 17-19 degrees. Could that be slowing my Wacker, leaving safrole unreacted? How should I heat it to fix this problem, if it's the source?

I'm doing all of the extractions and washes beatifully. I don't think the problem's there.

I'm getting so goddamn frustrated. Also, the lavender ketone does smell like pepper, and it's not much volume, but it is like 25g. Is Ketone more dense than safrole? What else could I be doing wrong?

posted 12-05-1999 11:53 AM         

Okay yeah you certainly need a *real* sep funnel (apologies to Strike who we know feels otherwise).

As to the temp in your "lab", I assume you mean 17-19 celsius... around 62 degrees F? No, not cold enough to interfere. That's not it. I know you don't mean 17-19F... no one would work in a room that cold. It seems to be pretty well-established that the conversion from safrole to ketone can happen at room temps, that is, it does not need heat to be applied nor does it need to have some exothermic heat generated (although with DMF as the solvent, this certainly does occur) to work.

I don't know what you mean by your distillation temps are "inflated" now that you're insulating the glass. They should be *decreased* (deflated??). Tell us what you're doing to stir the stuff in the flask (if at all; that would be a big factor if you weren't), how you're heating it, what type of vacuum you're using, how you're sealing your joints in your distillation setup, etc. More details will get you more help.

If I recall from your prior post, it sounded like you were doing the wacker correctly, you had all the right colors etc., but if as you say a LOT of safrole came over, that means your conversion was majorly incomplete. When you do a wacker well, you should get only a tiny, insignificant amount of safrole. So you will need to examine your technique doing the wacker also.

Sounds like mainly though, you're going through growing pains learning to distill. I'm going to take a wild guess that you have NOT spent long hard hours studying the posts in the Hive archives that talk about distillation. You have to do this. Do it now, before you go any further. Spend, oh I don't know, say 12 hours reading that stuff, or however long it takes you to read ALL of it. Then read it again. Read it until you're mumbling about vac distillation in your sleep. If you have never been taught by another human in this, this is what you must do to understand this deceptively simple task.

Lavender ketone, eh? Weird color... sounds like you may be talking about the reddish color that the wacker reaction produces. At any rate, it's totally impure, so dump it back into your mix (assuming you didn't polymerize or otherwise cook the stuff left behind in the flask too much) so that you can try again another day. By the way you are using a high-BP buffer oil mixed with the raw ketone (reaction mix) to prevent scorching, aren't you?

I'm tired... someone else take over helping this fine young man...

posted 12-05-1999 12:07 PM         

Quirks is light years more seasoned than me, listen to him before me. Personally though (assuming you are talking about the benzo wacker), I wouldn't attempt amination until I was convinced the ketone was reasonably pure (light neon yellow-green from the benzo wacker).

The question of temperature in wacker oxidations is an interesting one indeed. Pressure wackers done with O2 and air in metal vessels create no apparent heat and yet have worked. Perhaps with the benzo variation there is a need for heat in order for the benzoquinone to attach the oxygen to the structure.

I don't like to disagree with a veteran like you, quirks, but my personal work ethic says "learn to vac-distill the intermediate product properly bee-fore moving on to the next part." The further he goes without knowing for sure he has things under control, the more unanswerable questions will pile up and create an unmanageable situation.

Just my $.02...

posted 12-05-1999 12:59 PM         

I dream with a corning hotplate/stirrer, 24/40 glassware (2 500 mL RBFs). I only have a 1.5"x.375" octagonal stirbar, but it does the job nicely. Some of my joints are sealed with vaseline, others aren't. Whenever I use vaseline, the joins just don't hold together like they should. It seems to be more dangerous that way than unlubricated. And I use EXTREMELY little vaseline. My vacuum is a Gast pump...no aspirator!! thanks God. In my house, the water pressure is halved by a flushed toilet.

Next...Before I did the insulation, I dreamt that I pulled saf over at 135. After insulation, I was pulling it over at 170. Bizarre, eh? Maybe my vacuum's fucked or isn't sealed, but my insulation is VERY VERY good. It's ceramic fiber insulation, and it's much more efficient than foil or what have you. My logic was this: Since temp is measured in the still-head, insulation would cause there to be much more heat around the thermometer bulb, thus increasing temperature readings. The temp of the actual flask and the setting on the hotplate has remained the same for before and after insulation. Does that make sense?

The Wacker Process I'm using is the exact BS recipe w/ more DCM/NaOH washes because I wanted cleaner stuff.

Am I more clear now? I just wish I could dream like, ya know, just 20g of ketone. That's ~15g MDA...and I'd be set, ya know?

posted 12-06-1999 10:50 AM         

Allow me to share how I, at least, get perfect vac every time. I use teflon tape---NOT the white stuff---rather, the thicker yellow stuff used for natural gas lines. I love the shit. You cut off a piece about 12" long (assuming 24/40 joints), and wrap it around the inner joint in a slightly overlapping spiral starting at the narrower end. Do not stretch it at all; just wrap it in an orderly symmetrical fashion. Then push the outer joint of the adjoining piece on there very firmly, easy at first then increasing the pressure til it won't move anymore. If you wrapped the tape in a single piece (you'll get a leak if you try to do it with two or more pieces) and a clean, overlapping manner, I guarantee you those babies will have perfect vac seal.

Try it, you'll like it!

posted 12-06-1999 05:47 PM         

Your yellow gas line tape deal sounds a hell of a lot better than the expensive teflon joint sleeves.

posted 12-07-1999 03:27 PM         

Peace...AB

OBTW, Methyl Man, you sure have come a long way in a short time.

posted 12-08-1999 12:26 AM         

I owe it all to the Hive. Never would I have learned so much from books alone. It's all about the dialogue. It gives one the courage to go ahead and try things, because one knows that that interaction will be there the next day to clarify the mysteries.