BS benzo wacker questions.

[hsark]

Yes you can use boiling stones but run the risk of hot spots and ruining your ketone. But like pots and SWIM are saying a stirring/hotplate will fix that prob. And the boiling stones dont help as much with even heating. Therefore you get much more bumping....

[XrLeap]

yeah, SWIM's next procurement will be the very much needed stirrer/hotplate.

[XrLeap]

Thanks everybody,

SWIM has got his magnetic stirrer and hotplate. Did amazing thing for his dream of MDP2P, got some safrole looking(clear) oil over from 120C(which safrole came @ 90C). When it reached 150C, it started to have slight blue tone, but was very clear.

As for his NaOH washes, he had many incidents of not able to see the layers forming, could be due to too dark. So, he just guess the amount to be left in NaOH, then add another round of NaOH, a more visible tones were noticed. SWIM's a happy man, but starts to dislike this dirty wanker, oops, wacker oxidation.....

[OcoteaCymbarum]

If you seem some blue, then its impuritities in in.
If your safrole comes over at 90, its about a 9-10mm Hg end vacuum, so your ketone should come over at around 128 celcius.
To me, collecting a product over a 20 degree range is too much, as many higher boiling products would come over.

I've run many wackers before. Since I tried the performic with Chromic's HCL hydrolysis, I'll never run the wacker ever again. My first ever performic got me a 77-78% yield (molar, not weight to weight, which is even better)from isosafrole. A wacker produces a bunch of side products such as Md1P2P, chlorinated products, I even wonder if it can overoxidize MDP1P to the carboxylic. As such the distillation is not as clean as with a performic. If you can get your hands on formic acid, its a real charm