VERY interesting literature on the wacker

[lab_bitch]

The one thing that I don't understand, is why it works in the patent.  There must be something that we are overlooking.  What yield did you get with cocatalyst?  My highest was ~40%.

[lab_bitch]

I might know why that last rxn I ran was so fucked up.  I had buried the safrole in the woods for about two weeks with some other chems.  During this time, toluene left over from a nitro amination leaked everywhere along with a little of the safrole.  The safrole smelled awful, nothing like the freshly distilled shit.  I'll try the same procedure again with pure safrole.

[Ritter]

Lab_B,

Why don't you use IPA nitrite instead of that crazy- volatile ethyl nitrite?  I think it would make life easier dealing with a reagent thats at least liquid at room temp!

[blaztoff]

My old partner used to swear by the methyl nitrites. He loved it and he would get extremelly high yields upwards of 65% every time. Personally I never put enough attention into it and didnt have enough experience to really tweak with it. Damn I wish I could get in touch with him on this-but he is of doing a world soul searching or something and a little hard to reach. But I do have tons of notes on it-all of his notes to and they might be of some very good interest.

Ritter are the ratios of rxn for the IPA comparable to the other wackers? I havnt had any info on it but i would assume it would be similar. How about H2O.
 
Lab bitch- the wacker Swim ran was a version of said partners H202. It worked and was second time it ran with decent results but something dosnt look right after animation. Will do a test next week when Swim has access to a library.

[Sunlight]

Lab_bitch, if I remeber correctly I got a 35 % or so with cocatalyst and probaly a 1 or 1.5 % of PdCl2.
Blazztoff, I got that 65 % but without cocatalyst and that 4.5 % of PdCl2, do you know how much PdCl2/CuCl2 did he use ?

[blaztoff]

I have to check those notes. But If I remember though he was tweeking it out and before he went on his soul search he was getting way higher. I preety much stayed to hydrogenations of his wackers and he is a genius on this. To bad he never trusted new fangled computers as he would put it. So I have to pour through mounds of his scribble and make sense of it. The nitrites where his baby though-it wasnt a norm but his pet project. Am currentlly going through his stuff and piecing it together for research of my own. But slow going since I dont have much time with my wife beating down my neck cause im supposed to be retired.

[Sunlight]

Nobody doubts you are retired, say your wife it's just documentation, science  

[Azarius]

Not related to the Wacker, but am I to understand from this thread that straight 10% Pd/C would bee a quick and effective catalyst for the isomerization of olefins such as safrole?

[blaztoff]

Sunlight I have went through some of his notes and found out some. Some of his notes are in Japanese though and I have no idea how to decipher those characters. But I have found one experiment that was preety much complete. It mentions using Bischloronitropalladium as the catalyst. He always said that the methyl nitrites were the future-he was jumping for joy when I landed him 4l of acetonitrile to play with for them. I did not pay attention to much to these experiments for these were not suited for any real production. I know everything is in his notes-he was real good at bieng cryptic with me and made me figure out what I should have known. It took me 2 years to figure out the proper catalyst for hydrogenations that we were using.
I dont have all the notes here but been meaning to get them. But only can go through them at work cause my wife sees them she throws shoes at me. Shes Puerto Rican and you dont piss them of.