This camera doesn't capture the color.. If you look at it in the light it is neon yellow green like Mountain Dew.

I used a Leybold Trivac d8a rotary vane pump at 1x10^-4 torr -- the Ketone distilled through a vigreaux at 126c. This pump will distill safrole at 88-95c
Also, I have a bit of safrole in the freezer and the ketone. The safrole is frozen solid, the ketone remains an oil. Looks very pure.
The smell is exactly as you have described, and the viscocity is quite different than safrole.

LOL

I got the pump used for $700.00. It needs to be re-sealed because of a stupid mistake with an HCL bubbler and a needle valve I set up...

I wanted to have enough vacuum to run multiple lines with strong vacuum. I can rotovap and distill at the same time with strong vacuum.

It sells new for about $1700.00.

I'm going to perform the Hg/AL amalgam this weekend.

I've read this whole rhodium archive on HCL gas generator methods.
https://www.erowid.org/archive/rhodium/chemistry/hclgas.argox.html

That write up claims that the method I've used before (dripping HCL over H2so4) is the best. Yet most of the Methyl Man write ups I've seen and other write ups for working with the Toluene base extraction, post amalgam, use the h2so4 over table salt style generator.

Why is this? Is there any advantage to using the table salt generator over just dripping aq HCL onto 98% h2so4 ?

Thank YOU!

_Pbint_

That write up claims that the method I've used before (dripping HCL over H2so4) is the best. Yet most of the Methyl Man write ups I've seen and other write ups for working with the Toluene base extraction, post amalgam, use the h2so4 over table salt style generator.

Why is this? Is there any advantage to using the table salt generator over just dripping aq HCL onto 98% h2so4 ?

Argox was working on a much larger scale than Methyl Man 

I was pondering as to why some aminations of this compound are yellow and ones from amalgams are clear...

Other colors such as reddish amines have been reported as well  Impurities from the method used to produce the ketone can be present during the amalgamation and react to produce such phenomena    This has been discussed many times on the Hive, but of course most of those threads aren't available anymore    The end results from the effort applied 

40.06g MDMA hcl from 50g of MDP-2-P recrystallized to 38.89g a la Methyl Man's variation of Ritter's amalgam. Only one small variation.. I used Mercuric Nitrate instead of Chloride... This keeps the reaction under control but it takes longer to kick of the amalgamation.

Really great reaction!

Bioassay == unqualified success as I type!!

w00t!

 

very good pbinteger. so how do yo like the end product and how do you rate the performic route overall?

glad you had a good experience with it. I also tried it with my fiance in December and it was amazing. I recrystallized it in boiling acetonitrile. There are pics posted on another forum. What solvent/s did you use ?

For the amination i used Osmium/Brightstar's with methylamine. Since I could easily get it I preferred it so that the reaction was more controllable and indeed it was. I used foil with thickness of 20 microns. I'd like to try using pie tins with thickness 75 microns and see what happens once.

well my point is that they also take up less volume in the flask ...when i get there I  ll let you know. Now I still have to process a bunch a raw material when i get the chance

Thank You

I've been refining my technique! I just finished another batch of MDP-2-P and the yield was 90% of isosafrole. I made some improvements.

It is imperative that you back wash your aqueous layers several times very thoroughly after the NaOH wash of the ketone. A LOT of product gets stuck in the aqueous layer after the subsequent water and brine washes.

Also distillation of this stuff needs to be done at the lowest temperature possible or you get a bunch of tar towards the end which reduces yields as well. So I just very slowly raised the temp inching up the variac bit by bit until it was dripping slowly through the condenser. It reduced the tar a great deal. Bee sure to insulate your fractionating column too....

I'll report yields of my latest run in a couple of days.

pbinteger, what do you mean backwash aq layer? can you elaborate on the exact procedure you followed?

He's saying that after washing the ketone/dcm layer after the rearrangement, to not throw out the washes you do on the layer. Reason being you can extract the washes with a nonpolar to get out the product which absorbed into the water durin the washes. Increasses yields as your saving every drop of product you can.

Hope that helped.

ImA