MDP-2-P and NAI

[Rasputin]

Hello all
Having some left over NAI from an HI run, I decided to give the MDP-2-P purification via NAI a whirl. It seems pretty straight foward except for one small thing, The write up just says "60gr dirty red ketone", does this mean unwashed ketone by itself not in DCM, or do I take it up into DCM and perform the washes as usual, then do the NAI step. I honestly cannot fathom not washing my goods, but I dont know if the DCM will will interfere with the NAI part. I have searched, but there is not much info on the Hive about NAI, mostly its Bisulfite suff. I did find one post with this same question, but the responses were just ridicule for not using Bisulfite. So the question is still unanswered I really hope someone can help, I mean someone has to have tried this process. Oh, I almost forgot, Im using the Benzo Wacker(in case it helps answer the question better)
Thanks Bees

[Rhodium]

The write up just says "60gr dirty red ketone", does this mean unwashed ketone by itself not in DCM, or do I take it up into DCM and perform the washes as usual, then do the NAI step. I honestly cannot fathom not washing my goods, but I dont know if the DCM will will interfere with the NAI part.

It means that the ketone is to be fully washed, the DCM dried over a suitable drying agent like MgSO₄, and the DCM distilled off (just as in the usual purification procedure, minus the distillation). Compared with

the writeup by Hellman

(https://www.thevespiary.org/rhodium/Rhodium/chemistry/naicomplex.txt) I would strongly advise against refluxing the solution (if even possible), as the bp of MDP2P is way higher than that of acetone and methyl ethyl ketone, the ketones this procedure is modeled upon. Just heat to 75-100°C (flask immersed in simmering water).

Please report back your results!

[Rasputin]

Hi all
As asked, Im posting the results of my expirements with NAI purification of MDP2P. I did the "Time streamlined Benzo Wacker", following the directions exactly, all chemicals were of reagent grade. I did the HCL/H2O flood, and after twenty minutes a layer formed in the bottom. I took it off and added it to  solvent, as per the instructions. The first three NaOH washes(3/500 mls) came off jet black. I then proceeded to wash seven more times with NaOH, each time they came off orange. I then washed three more times with DH20(3/500 mls), they also came off orange, but it was a very lighter shade. I then dried with 40 gr MgSO4, for thirty minutes. I then stripped off the solovent. I took 60gr of the "Ketone", added 10gr of NAI, and heated to 100C for ten minutes. None of the NAI dissolved into the "Ketone". I put it into an ice/salt/water bath for ten minutes, still no change. I filtered off the NAI and washed it with a little(50 mls) Xylene( no Toluene available). After it was dried, I added it to three hundered mls of warm DH2O, shook, and nothing sepperated out. All of the NAI dissolved in the DH2O, but there was no "layer of Ketone".

My own conclusions: 1. The process does not work on MDP2P( I dont know why it wouldnt Ketones are Ketones right?)

Or

2. I dont have "Ketone", and its still just Safrole( In the freezer it never froze, it did get very viscous however, isnt that one of the charecteristics of "Ketone"?)

Im not a certified chemist, so I am truly puzzeled, if anyone has any comments or criticism( possitive or negative) Im open and welcome to hear it.

P.S. Rhodium: since your the only one that had any interest in my post, I would really like to hear your input most of all.

Until later: Thank you all, in advance.

[XrLeap]

hi, you may try NAI with acetone to see the effect first, then try it again with the ketone.

SWIX is very interested in knowing the result...... SWIX tried using sodium bisulfite for purification and it was quite dirty and obtained balck bisulfaite adduct. so SWIX is planning to try NAI. good luck:)

[pooky]

With the distillation you should have a good idea if you have ketone,as the boiling temp for ketone is much higher than saf.Rhodium has a nomograph on his site to get an idea.
P distills the raw ketone out of the benzo mess,and then re-distills that;when the temperature rises a few degrees, after almost all of the raw ketone is distilled,then it's good enough for P.Is almost clear,and will never freeze.Using this ketone with LaBTop's borohydride reduction always gets P 110g of freebase from 100g ketone.

P tried both of the chemical purifies and just ended up with huge messes and aggravation.

[Rasputin]

My assumption is that I dont have Ketone. I ran another Wacker last night, and Im going to work it up tonight. I will post my results, as soon as Im done. I am going to give this process another try(I hate giving up).

P.S. Thanks for replying, I knew I wasnt the only one who was interested in this process.

P.S.2 You said it never freezes, does it get very viscous for you, mine did.

Anxiously awaiting further replies