posted 08-03-99 11:56 PM         

All of you, and you know who you are, that posted this method, should be ashamed of yourselves,.
Your reasons for posting what you did, are crafty, but in vain,
I'd guess you had all wanted it to work, so bad that you thought that if you said it did, all the poor, poor bees would follow your broken chain, and hopefully prove this theory right,.
Sorry to burst you bubble LAbtop, tboc and the rest.

You can flame me as much as you want, but the fact remains, IT JUST DOESN't work,.

this is chemistry, not hopey,hopey land

for fucks sake

posted 08-04-99 01:54 PM         

And that just makes it so true. Oh, and there is no way in hell there would be anyone of that level/skill on this board; there just couldn't be. They would never do such a thing.

>It was part of my final year, freelance project.

I'm sure it was.

>All of you, and you know who you are, that posted this method, should be ashamed of >yourselves,. Your reasons for posting what you did, are crafty, but in vain,

Tricky indeed. I agree only slightly if this is true, but you'd have to admit, it was a good cause They must have pushed your buttons pretty good.

>I'd guess you had all wanted it to work, so bad that you thought that if you said it

Such selfish reasons that would never benefit us, would it? And there was never any sound hypothesis stating that it might possibly work, was there?

>all the poor, poor bees would follow your broken chain

Oh, you mean freeloader bees who can't think about it on their own, have no scientific background or skill to use their judgment and must let someone with 'credibility' do it first? I want it written up like the 'Bright Star' paper, please, please, wahhhhhhh! Free money, free money, I wanna be a punk and heat out the sources for anyone else in my neighborhood too.

>Sorry to burst you bubble LAbtop, tboc and the rest.

LaBTop never said it worked or didn't. Get your facts straight if you want to be credible. I'm sure tBOC's bubble is burst so bad that he doesn't come back. He'll just go enjoy what he knows he can do and run around naked on the street by himself.

>You can flame me as much as you want, but the fact remains, IT JUST DOESN't work,.

Oh, more scientific evidence. This helps.

>this is chemistry, not hopey,hopey land

Rats. I'm definitely in the wrong place. I wish I knew this sooner

Just keeping an open mind.

posted 08-04-99 02:15 PM         

If you should have read the following carefully, you could have known allready half way july that there were allready a few bees for whom it did not work. This is a bad sign, but does not mean you must give up hope. In my case, 3 years it did not work until I got it to work( another method!).
And by the way, I POSTED TO the thread, I did not POST it myself.
So carefull reading will at last reveal also to you that there was a LOT of doubt, but also a lot of willing to test it out, because if it works, its sensational, UNDERSTOOD? (Vade Retro, Satanis )

QUOTES:

Xeolite
Member posted 06-28-99 07:58 PM
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I think tBOC said enough and answered enough questions. If he stayed, the questions would never end. Perhaps it wouldn't be 'safe' or 'wise' for tBOC to return after his malicious blow to the DEA.
tBOC has given us more than enough info and the freeloaders are just waiting for others to confirm it when they should be contributing also. It is now up to us.

Postit
Member posted 06-29-99 01:08 AM
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I have not given up 100%, but even this was tested by some professional chemists and they came up with nada..... Search past posts. Did SWIM run a NMR or GC to test? Everyone from the hive that has had access to these tests came up dry. I am forwarding this to someone that does have access to NMR to get a final word on the issue.

Semtex Enigma
Member posted 06-29-99 01:43 AM
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The only test(s) were smell and bisulfite, sorry don't have access to the rest...

sunlight
Member posted 06-29-99 03:11 AM
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Smell and bisulphite are not enough. Ketone has differents smells depending on the way it comes from, always it has imputities that make the smell be different. And bisulphite addition can be done with aldehydes. My oppinion is that if not analytical confirmation can be achieved, the only way is to make an amine salt, biological test and melting poiint, and even this is not complete.

Xeolite
Member posted 06-29-99 06:19 AM
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I think we've got enough info to at least give it a try ourselves instead of wait for someone to do tests (for those who are eager to do a taste test . We have the person who did NOT run around naked on the street (a great test), and we have the chicken fat from someone else. I've got everything ever spoken of this copied and pasted and I see no 'pro' claiming poor results, eh? Postit? Lots of support by theory and knowledgeable people though. tBOC even posted the original ref: JACS Vol 70, pg 3666 (1948).
Oh, and Semtex, the thread I was speaking of was Piglet's posted 06-02-99 06:24AM

"...secondary alcohol from terminal alkene has been proved...the compound converts to the 1-ol so readily, I propose that the group moving the other way is VERY unlikely...an aldehyde would test positive, and I remember the palladium acetate thread only too well...in this case, I would bet that if you get a positive bisulfite, then you got your ketone. If the 1-ol oxidized, the addition won't happen."

Postit
Member posted 06-29-99 12:21 PM
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I do know that mdp2pol is formed by mixing a cold 70 - 80% H2SO4 solution with cold safrole. BrightStar did confirm this with IR and NMR I believe. But the stuff migrates to mdp1pol very quickly and no one has been able to oxidize it to mdp2p. Mabe BS can confirm this faster than me since he does have the right equiptment. I believe 100% that it CAN be done but am not so sure this method works........... I am a scientist and live off of skepticism. I want to be proven wrong. Believe me it would be an answer to many peoples prayers. Once it is confirmed that it has been converted to one of the ever loved MD analogs then I will issue a large congrats to Tboc and everyone else that has worked on this.

Xeolite
Member posted 06-29-99 02:10 PM
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How about this, let's all stop beating tBOC for answers for now and next week I'll tell you guys of a hypothetical procedure related to this one (all ACS grade will be used), scaled to 800g safrole and whether it fails to yield 'something' or not. No tests other than the tests of as many running around the street naked as I can get and that is it - and whether they think it feels different than the quinone/NaBH3CN reduction product!

LaBTop
Member posted 06-29-99 05:37 PM
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WELL SAID, Xeolite, lets cut the crab!
Some willing friends with more then normal interest in this procedure will contribute to this too. ( I heard a rumor they had a SHITTLOAD of Saffrole oil 98% laying around somewhere). They will also concentrate on this one.

IF positive, tBOC will get all the Fame he can carry!! I promise you personally!

F_CKIN SH_T D_MMN_TT MF'IN MORONS.........! LT/

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EMOTIONSwill always beFREE!

LaBTop
Member posted 06-29-99 05:54 PM
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One little remark:
You ever tried to put Water in conc H2SO4?
And NOT the other way round!
Saw or FEEL the EXOTHERMIC reaction?

MORONS

LT/ :abitpissytoseeagoodlookingprocedureendbad

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EMOTIONSwill always beFREE!

Xeolite
Member posted 06-29-99 09:18 PM
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Do as you oughter, add acid to water!

Semtex Enigma
Member posted 06-30-99 02:15 AM
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I thought it was like alphabetical, you know add Acid(s) to Base(s).?. :0

Osmium
Member posted 06-30-99 03:50 AM
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O. is sceptical about this procedure, too. In the past, I was one of those who said it would not work. Now, if that really works, I'll be happy just as anybody else. tBoc and whoever was involved, I'll kiss your hairy asses, with tongue and all, please confirm that this does not produce the propiophenone, aldehyde or whatever.
The propiophenone is a solid, but the melting point is rather low. To test for the propiophenone, a chromatographic purification should be used, followed by storage in the freezer. Or dissolve the product in the same amount of hexane and cool it with some dry ice. I solids appear, chances are high it really is the propiophenone or aldehyde or something else.
The product from the amination of this supposed ketone should also be tested in vivo, and don't forget to test the melting points of this amination product, pure MDMA made with another procedure, and of course the melting point of an intimate mixture of both substances. If this mixed MP is depressed, the product can't be MDMA. Using comparable crystallisation procedures, maybe followed by a recrystallisation from the same solvent are of course necessary here.
Another good test is producing some solid derivative (like reacting with dinitrophenylhydrazine) of the supposed ketone and compare that to the one made from authentic MDP2P. Please, somebody out there with the resources, that's a few hours work and all the questions will be answered. If I had the resources, I'd do all that, but unfortunately, I can't.

Osmium
Member posted 06-30-99 04:02 AM
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Another way to test for methyl ketones is of course the haloform reaction. Somebody please do all the necessary tests and write a detailed paper!

Xeolite
Member posted 06-30-99 05:05 AM
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Noooooooooo! Not you O. Darn I wish I knew you didn't like this before I hypothetically purchased materials. Why do you not like?

ymir
Member posted 06-30-99 08:41 AM
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For those bees of limited resources, the old Vogel's has a diagram of an improvised melting point test apparatus made from a flat iron. Loki's variation is made from a flat iron sitting in a coffee can, plugged into a 1500 watt rheostat, with the probe of a pyrometer held next to the sample by soldering stand. The iron's heat control is turned all the way up, the heat is slowly raised with the rheostat. It works great!

Labrat
Member posted 06-30-99 09:37 AM
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Maybe a few tips would be handy so this procedure can finally be put to work:
Adding the acid to the alkene creates a lot of heat, reversing the addition obviates this problem and keeps polymerisation to a minimum. Thus, add your alkene slowly and dropwise to the acid. The color should progress from light/brown to deep red. Diluting the acid can be done in the same way (so add the acid/alkene mix to the water). The color change you'll see here is from deep red to pink and finally a whitish kind of milky mix.

It seems that heating over 55 C during oxidation makes the mix go brownish/black all the time. This might be different with other people, but keeping the temp low is important! Hopefully someone here can make it work, I couldn't. Good luck! Lr/

Osmium
Member posted 07-01-99 03:52 AM
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Xeolite: I always argued that the benzyl alcohol will be formed in this reaction. I still believe that this is very likely, but many other bees (including drone and his Beilstein account) say that this not the case. Please let's not start this useless discussion again, the proof of the pudding is in the eating. Somebody out there do all the necessary steps, it's really not much work for an organic chemist, and post your results.

Xeolite
Member posted 07-02-99 01:20 AM
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Well said
A few more days...

r2d3
Member posted 07-02-99 10:09 AM
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Well here we go again. In this thread the current score on the mixing of the alkene/H2SO4 is Acid to Alkene 4 (LaBTop, S.E.,P.S.,tBOC) and Alkene to Acid 2 (Labrat,Micr-O....). Does this remind anybody of the modified performic, and the sodium carbonate? I will only vote in the case of a tie.

Semtex Enigma
Member posted 07-03-99 07:58 PM
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As long as it works, personally i'd (i'd NEVER acually do this, cause that would be BAD) do as tBOC suggests and add the acid to the olefin. Then you add the water, you'd never even have to adjust the addition/sep funnel. If one did it the other way one has to remove the acid/olefin mix from the flask put the water into the flask and then try to keep the acid/olefin mix cold while dripping from a sep/addition funnel which to me doesn't sound practical for scaling up at all, the 20g batch might get too warm while your dripping proceeds. Sorry for the run-on sentence...

Semtex Enigma
Member posted 07-03-99 08:04 PM
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Opps, forgot.
LabRat: SWIM has noticed that adding acid to olefin as tBOC described does result in a browny/blackish looking mix. However after addition of the water at the same rate the acid was introduced(1drop/sec)the mix turns a milky pink, like watered down strawberry quick. After seperation the water layer is milky, but the alcohol layer is clear pink/reddish. No tar, no polymerisation (I know it ain't spelt right!!!) just pretty pretty alcohol, or so I've been told...

Postit
Member posted 07-09-99 10:31 PM
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Xeolite - Its been 7 days, so what is the verdict? Just got back online and was wondering.....

Semtex Enigma
Member posted 07-09-99 11:45 PM
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I was told that Xeolite had to goto a wedding or a party for the weekend, he might not answer till monday or so...

Xeolite
Member posted 07-10-99 02:11 AM
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Yeah, you'd better believe it!!! It's not 'till during the reception when everyone gets fucked up

Xeolite
Member posted 07-10-99 02:42 AM
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Oh, and the wedding that I am going to is the wedding of the Brotherhood Of Chemists!
tBOC's!? ;D

Semtex Enigma
Member posted 07-10-99 04:48 PM
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Is that one of them good old boys clubs? Sounds pretty exclusive...

Micr-O-NNN-2
Junior Member posted 07-12-99 05:03 AM
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Here again. Heard one clone or other trying this AGAIN.. this time adding acid to alkene.
Well. That part works. he got what he thought was alcohol, small almost clear- a bit yellowish layer on the top of milky pink liquid (he just loves dry ice). Onwards with oxidation - screwed. when the temp rises, the solution turns brown-black. And it's not looking healthy he tells me. No product was recoverable from the gunk that was produced. This happened definetily before solution started to reflux, so-oo.. what's wrong? Isn't it supposed to reflux? All reagents were Puriss or better.
Clone is starting to get a bit pissed off. All wasted alkene and credits, not mentioning the time.

So? Am asking again. Is anyone able to confirm that this works? If not, this clone is going to revert back to old methods which have been proved many times.

I'm not saying this is all crap. it still might work, tBoc and Semtex are claiming success. But either clone has very bad lab-technique or there is something fishy going on.

Well, it's my job being paranoid so whether this works or not this is not going tobe tried in Complex before someone can give some definite data. Xeolite?

Clone is starting to bit

Getafix
Member posted 07-12-99 06:11 AM
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Someone also tried this. Added the acid to the oil. Turned dark purple-black. When water was added a light yellow-white layer separated out. The oxidation with excess acetic acid resulted in volcanic eruptions of brown, vinegar smelling shit. Happened twice.
The original formula was used with a small amount of acetic acid. This refluxed nicely and a yellow oil was obtained. Had a slight tinge of red, but the fluorescent look was missing.

Amination was attempted, but failed completely.

So back to Benzo-quinone wacker it is!

-getafix

Semtex Enigma
Member posted 07-12-99 05:19 PM
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Just a note, Semtex's buddy SWIM NEVER confermed FINAL results. SWIM did the proceedure and everything seemed to go well, however the ONLY test that was done on the resulting (?)ketone(?) was a bisulfite test, which it passed. But we all no that it is not a difinitive test, SWIM is not able to "play" right now, so he/she hasn't been able to try to aminate the result of tBOC's little proceedure.
Another thing, SWIM noticed that some of you are getting alcohol(?) and then it's the next step that screws up. Make sure that you add everything to the alcohol while it is still in an ice bath, THEN heat GENTLY, like 1/5 power on SWIM's hotplate. I think you guys might be heating for too long or perhaps too hot, swim never saw no black shit, just had a nice blue hue to it from the CuAc...

Keep up the good work on this people, for if we get this to work we'll have already won...

Osmium
Member posted 07-13-99 06:30 AM
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(Somebody really should test the bisulfite thing with some propiophenone... Solids? No solids?)
Anybody found an old bottle of propiophenone in his garage recently? If the answer is yes, could you please add some to bisulfite solution and tell us what happens?

Semtex Enigma
Member posted 07-13-99 06:57 PM
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I think a bee with a better equip'd garage will come forward in the next few days, I hope anyways...

I sincerely hope YOUR garage was well equipped, so give us the juicy details instead of beginning a flame war yourself with NOT ONE detail of the test! LT/

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EMOTIONSwill always beFREE!

posted 08-04-99 10:21 PM         

I will say it again,
The proceedure, well all proceedures here, detailing the h2s04 bullshit do not work,
If you are trying to sneak out of this one by saying that you have a different method, let's see it,.
I know what you are doing, and it stinks.

So you know say that you got it to work, but only with another method, and after 3 years of practice, well, thats quite a story.
Isn't it,.

Titanium- Get a life, you don't even know what your talking about,
Brightstar nmr showed p2pol, not mdp2p,
NOBODY, NOT EVEN THE GREAT RHODIUM,OSMIUM,STRIKE or anybody has got the ketone,.

The problem here is to change this highly, highly unstable alcohol into a ketone, I don't know how, but then again, nobody here does.
Ammonium salts will burn the living shit out of it,.
You're gonna need a stabilizer, a softer smoother oxidiser, and take it through a few more steps after you have the p2pol,
You have to first alter the the p2pol, not by oxidising it, but by rearanging it somehow,
I DON'T know how.

hellman
Really, all I am trying to do is help poor bees from these traps that have been set by more well respected bees-this excludes Osmium,Rhod's,strike,As they have never claimed its success.

If you don't like my opinionated facts,
prove me wrong

posted 08-04-99 10:25 PM         

Can you spell guilty,.
Why did you waste 5 pages of pasted diatribe
on defending something which you have got to work,
Hmmm, bees- read and enjoy.

posted 08-04-99 11:12 PM         

??? Proceeeeedure??? What method did your prof use??? Who's proceeeeedures???
When you say H2SO4 bullshit, that will automatically make people think you are speaking of the saf+H2SO4 -> alc Well, the AcOH reflux does stick, I'll agree with you on that

>So you know say that you got it to work, but only with another method, and after 3 >years of practice, well, thats quite a story. Isn't it,.

I think LaBTop is speaking of a different method of something completely different. The reduction with the NaBH4, right, LaBTop? Read more carefully hellman.

>Titanium- Get a life,

…speechless. Ouch. Especially coming from you, boss.

>you don't even know what your talking about, Brightstar nmr showed p2pol, not mdp2p, >NOBODY, NOT EVEN THE GREAT RHODIUM,OSMIUM,STRIKE or anybody has >got the ketone,.

THE GREAT? I hope that is not sarcasm. Bright Star showed the H2SO4 product which was the alcohol and you stated that the H2SO4 'method' doesn't work. What the fuck is the oxidation you're talking about with H2SO4, oh, you must mean the AcOH/Cu(Oac)2/alcohol one. You don't know what you are talking about, buddy. The only person who said they got the ketone so far is tBOC and I don't think he gives a flying fuck about people like you judging him whether he was mistaken or not and I don't recall him doing and nmr on the shit either.

>The problem here is to change this highly, highly unstable alcohol into a ketone, I don't >know how, but then again, nobody here does. Ammonium salts will burn the living shit >out of it,. You're gonna need a stabilizer, a softer smoother oxidiser, and take it through >a few more steps after you have the p2pol, You have to first alter the the p2pol, not by >oxidising it, but by rearanging it somehow, I DON'T know how.

I don't think anyone would disagree with you much here except for tBOC or anyone else who has done it.

>Really, all I am trying to do is help poor bees from these traps that have been set by >more well respected bees-this excludes Osmium,Rhod's,strike,As they have never >claimed its success.

Well then stop wrongfully accusing anyone and acting like an asshole with no scientific method backup just because you lost some chump change in your bad experience and want to cry about it.

>If you don't like my opinionated facts, prove me wrong

I sure hope someone does.

>Oh labtop, Can you spell guilty,.Why did you waste 5 pages of pasted diatribe on >defending something which you have got to work, Hmmm, bees- read and enjoy.

I'm sure all bees would take your word over his any time - NOT. It's not wasted space. LaBTop 'might' be nice enough to try to tell you something.

posted 08-05-99 01:51 AM         

The one and only reason grandaddy even likes this new procedure isn't because it uses easier to obtain chemicals, but because if the bugs were all out, you can get away with ketone with no extracting, washing and distillation. If these things are needed, to him it isn't worth it and he'd rather do it old school. Daddy will try again soon maybe and has friends that may in China.

For reasons I'll take to my grave, I believe in tBOC 99.9%, but still have yet to see anyone get the bugs out.

posted 08-05-99 02:42 AM         

Reminder: tBOC had many, many fuckups too and described them. Many details of a lot of the reaction are exactly as he described.

posted 08-05-99 03:21 AM         

Are you saying that the final aminated product was inactive, or did it show unsuspected pharmacology? Sedation, maybe (=sleeping party)?

posted 08-05-99 03:55 PM         

"I know what you are doing, and it stinks."

Does mister wise guy think I'm enjoying a MeNH2 synth now? Yep, could stink if you use your skills and brainpower......
But I'm in fact smelling some nasty character twists here, if I'm not mistaken.
You still do'nt even BOTHER to READ, so, you have some possibilities left:

1.Read.
2.Could it be that your interested in making ketone, but up till now could'nt manage yourself to bring it up to read the OnePot NaBH4 threads(5) for amination of said ketones, where I mentioned it took me 3 years of bitter trying, before I was satisfied?
"TO AMINATE KETONES", dislectic moron !(sometimes it feels justified to call some names, I'm getting the grip of it )
AND that's what any sane person can see when someone EXPLICIT mentions "another method".

3.And where did I ever "claimed its success"?

So you ranter a lot, but where are the bare FACTS?
And again, it looks more and more that it will not work for most of you, but "God" created only one Einstein and one Mdm. Curie and one Stephen Hawkins, and luckely only one Hellman.
"Vade Retro, Satanis !" LT/

PS: I'm not "actif" anymore, so someone else will get the honors, if/when he/she can ever mirror the results written down by tBoc.
And if he's a fraud, then he damned well know how to post a few goodlooking write-ups, which skill you at least, lack, obviously too busy with egocentric activities.
And he left no home address for you, to confront him with your anger; wise guy(tBoc)
PPS:
don't get me wrong hellman,
I still love you,.
And your a damn ****** contributor,.
LaBski

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EMOTIONSwill always beFREE!

posted 08-05-99 04:16 PM         

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EMOTIONSwill always beFREE!

posted 08-05-99 06:04 PM         

That's odd. At least at my school, I've never seen a professor so much as pick up a beaker (that's what RA's are for), let alone do someone's "freelance project". How did you manage to convince a professor to do this for you?

What procedure did this professor use, and what were the results? We need details! Also, why is it that you believe this experiment that witnessed proved unequivocably that hydration of allylbenzenes doesn't work?

There seems to be some confusion in the wording of your post, which leads me to believe there has been a communication breakdown. You talk about getting the ketone from safrole by doing some sort of oxidation involving H2SO4, but I have yet to see a procedure fitting this description. Either you're being a little too free-and-easy with your chemical shorthand, or you're misinterpeting what was postulated. Many people have mentioned H2SO4-catalyzed hydration of safrole, but this is not an oxidation. What are you saying, exactly?

I've posted refs upon ref's of examples of successful hydrations of methoxylated and methylenedioxylated allylbenzenes - inculding safrole. Use the search engine, and you'll find them. Either those of us with success with this method, as well as the folks who wrote those articles are all jokers, or you may be wrong.

I don't know what else to say.

posted 08-08-99 10:49 PM         

the facts- noting more nothing less,

1) tlc results of adding conc h2so4 to safrole 78% mdp2pol
2) tlc results after oxidation with ammonium salt 0% mdp2p
3) done in university lab with 1-decene, by lecturer.
4) done in clandestine lab with 99.8% safrole by TLC with similar results.
5) I do not read all posts

opinions

1) I believe it is possible, it JUST IS NOT by the current success posts delivered here to the hive by you know who( So if that's not you, don't stress O.K.)
Don't how a cow man, in other words.

flames.

1) Tits-analiam- leave me alone, you now do not have my permission to speak to me.

2) Labtop- Just love ya!

responses.

1) droney-yeah i know, it should work, I am pretty sure it's as simple as finding a more selective oxidiser
2) Labtop- If only the borohydride was OTC,.

Conclusions.
now that we all have ketone basically sussed by previous working methods, peracid,pdcl2.
We should now strive to make it just a little easier, by this I mean easier
1) glassware,
2) easier methylamine,
3) easier purification

Shouldn't we strive to have a synth that at least doesn't use glassware, isn't that what we are all about,.

posted 08-09-99 05:57 PM         

Anyway, I would like to suggest that trying to make MDP-2-P from the 2ol compound might be a bit too linear (conventional) thinking. There is a thread going in the chem forum on making a TOSYL or MESYL compound from the 2ol. I personally have been contemplating the nature of a triflate derivative of 2ol. The mesyl and tosyl chloride (or anhydride can work) reagents in this reaction are cheap and easy to acquire (in most places, how could they *ever* become watched chems???). These derivatives are *theoretically* aminated in high yield. It is similar to, but far superior than, the iodosafrole route.

Anyway, I know this is a bit of an aside, but I was hoping to get some of the chem knowledge in this thread to peek in at the other one. And, after all the goal is to find better methods (I agree that the refs seem to suggest this works and will be a potentially useful synth, but you can't stop progress).